Palladium Sample Clauses

Palladium charcoal (5%) until the absorption of hydrogen had ceased. The catalyst was filtered off and the filtrate evaporated to dryness. The residue was taken up in 5 ml. 2N hydrochloric acid, cooled to -5 degrees C. and treated with 2.5 ml. of 10% aqueous sodium nitrite solution. After standing for 30 minutes, the clear solution was added at -5 degrees C. to a solution of 0.5 g. salicylic acid in 20 ml. of a 1N aqueous sodium hydroxide solution. After subsequently standing for 3 hours at 20 degrees C., the reaction mixture was acidified and extracted with diethyl ether to remove unreacted salicylic acid. The aqueous phase was adjusted to pH 7 by adding 1N aqueous sodium hydroxide solution and the resulting solution was evaporated to dryness. The residue was further dried by adding toluene and subsequently evaporating it and the residue then extracted with methanol. The methanolic solution was concentrated to a small volume. After adding diethyl ether and cooling, the disodium salt of 5-(4-(a- dimethylaminocarboxypentylcarbamoyl)-phenylazo]-salicylic acid separated out; m.p. (greater than) 210 degrees C. (decomp.).

Palladium charcoal (5%) until the reaction was complete. The catalyst and solvent were removed and the residue was crystallised from ethanol-diethyl ether (1:1 v/v) to give 4.7 g. 6-(4- aminobenzoylamino)-hexanoic acid; m.p. 132 - 134 degrees C. c) A solution of 2.5 g. 6-(4-aminobenzoylamino)-hexanoic acid in 15 ml. 2N hydrochloric acid was cooled to -5 degrees C. and treated dropwise, while stirring, with 8 ml. of a 10% aqueous solution of sodium nitrite. The reaction mixture was stirred for 30 minutes and then added at -5 degrees C. to salicylic acid in 20 ml. of water containing 2 g. sodium hydroxide and 1 g. sodium carbonate. After 3 hours, the reaction mixture was acidified and the precipitate obtained was isolated by centrifuging, dissolved in ethyl acetate, washed, dried and concentrated to a small volume. Upon cooling, there were obtained 2.7 g. 5- (4-carboxypentylcarbamoylphenylazo)-salicylic acid; m.p. 238 - 239 degrees C. Example 10. ----------- a) A solution of 13 g. copper sulphate in 60 ml. water and a solution of 2 g. sodium hydroxide in 30 ml. water were added simultaneously to a solution of 7.5 g. lysine in 50 ml. water, followed by the addition of 50 ml. of 10% aqueous sodium bicarbonate solution. The precipitated salt was filtered off and the blue filtrate was added, with vigorous stirring, to a solution of 7 g. 4-nitrobenzoyl chloride in 50 ml. acetone. The reaction mixture was stirred for 20 hours and the precipitate obtained was filtered off, washed with water, methanol and diethyl ether and dried in a vacuum at 50 degrees C. to give the copper salt of (E)-(4- nitrobenzoyl)-lysine. b) A suspension of 7 g. of the copper salt of (E)-(4-nitrobenzoyl)-lysine in 30 ml. water was stirred with 6 ml. hydrochloric acid until dissolution was complete. Hydrogen sulphide was passed in for 1 hour and precipitated copper sulphide then filtered off. The filtrate was evaporated to dryness and the residue was taken up in 20 ml. methanolic hydrogen chloride and heated under reflux for 3 hours. The cooled reaction mixture was diluted with water, rendered alkaline with sodium carbonate and extracted with ethyl acetate to give 4.8 g. (E)-(4-nitrobenzoyl)-lysine methyl ester in the form of a yellow oil.

Palladium charcoal (5%) until the reaction was complete. The catalyst and solvent were removed to give 5 g. N,N-diethyl-N'-(4-aminobenzoyl)-ethylenediamine in the form of an oil. c) A solution of 2.35 g. N,N-diethyl-N'-(4-aminobenzoyl)-ethylenediamine in 20 ml. 2N hydrochloric acid was cooled to -5 degrees C. and treated with 8 ml. of a 10% aqueous solution of sodium nitrite. The reaction mixture was stirred for 30 minutes and added to 1.4 g. salicylic acid in a solution of 1.6 g. sodium hydroxide and 2 g. sodium carbonate in 20 ml. water. After 3 hours at 0 to 20 degrees C., sodium chloride was added to the reaction mixture to salt out the desired diazo compound. This was filtered off, washed with water and hot methanol and dried to give 2.3 g. 5-(4-diethyl-aminoethylcarbamoylphenylazo)- salicylic acid; m.p. 252 - 254 degrees C. (decomp.). The pharmaceutical compositions according to the present invention contain at least one of the compounds (R&D Schedule 1 cont...) -20-

Palladium. During the Contract Year 1999, SMC will sell and --------- deliver and Ford will purchase on a monthly basis [***] of Actual Monthly Production. During the Contract Years 2000, 2001, 2002 and 2003, SMC will sell and deliver and Ford will purchase on a monthly basis [***] of Actual Monthly Production. The parties acknowledge that the Actual Monthly Production will vary from time to time. [***] [***]

Palladium. Ford will purchase up to [**Redacted**] Ounces of Palladium each month of the Term.

Palladium. During the Contract Year 1999, SMC will sell and --------- deliver and GM will purchase on a monthly basis [***] of Actual Monthly Production. During the Contract Years 2000, 2001, 2002 and 2003, SMC will sell and deliver and GM will purchase on a monthly basis [***] of Actual Monthly Production. The parties acknowledge that the Actual Monthly Production will vary from time to time. If, during the years 1999 through and including 2003, SMC fails to deliver to GM at least [***] Ounces of Palladium pursuant to this Agreement, then the term of this Agreement shall automatically be extended until such time as SMC has delivered to GM, at a rate of [***] of Actual Monthly Production, an aggregate of [***] Ounces of Palladium pursuant to the provisions of this Agreement.

Palladium. By: /s/ Xxxxxxxxxx Xxxxxxxxxxxx Xxxxxxxxxx Xxxxxxxxxxxx Title: Chairman [CORPORATE SEAL] [UNITED STATES NOTARIAL ACKNOWLEDGMENT REQUIRED] K-Swiss Inc. By: /s/ Xxxxxx X. Xxxxxxx Xxxxxx X. Xxxxxxx Title: President

Palladium. Palladium Communications, Inc. 000 X. Xxxxxxxx Xxx Boulevard Louisville, Kentucky 40202 Attn: Xxxxxxx X. Xxxxxxxxxx, Xx., President Phone: (000) 000-0000 Telecopier:

Palladium. During the Contract Years 1999, 2000 and 2001, SMC will sell and deliver and MIC will purchase on a monthly basis [***] of Actual Monthly Production. During the Contract Years 2002 and 2003, SMC will sell and deliver and MIC will purchase on [***] During the Contract Years 2004, 2005 and 2006, SMC will sell and deliver and MIC will purchase on a monthly basis [***] of Actual Monthly Production. The parties acknowledge that the Actual Monthly Production may fluctuate from time to time.

Palladium. The price per Ounce to be paid to SMC by MC for --------- the actual quantities of Palladium delivered during each month pursuant to Section 3 above shall be based on the [***] for the Pricing Month less a discount of [***] per Ounce. [***]