反应详情

To a suspension of N-tert-butoxycarbonyl-1-methyl-D-tryptophan (1.60 g) and hydrochloric acid salt of D-methionine ethyl ester (1.06 g) in dry methylene chloride (30 ml) which was cooled on an ice bath and stirred was added a solution of triethylamine (0.50 g) in dry methylene chloride (10 ml). The mixture was stirred for 30 minutes, and to the mixture was added a solution of N,N'-dicyclohexylcarbodiimide (1.04 g) in dry methylene chloride (10 ml). The resulting mixture was stirred overnight. After removal of the solvent, crude residue was taken up with a mixture of ethyl acetate and water, filtered, and organic layer was washed with 10% hydrochloric acid and saturated sodium bicarbonate solution, dried over magnesium sulfate, and evaporated to give crystalline N-tert-butoxycarbonyl-1-methyl-D-tryptophyl-D-methionine ethyl ester (2.43 g).

1. temperaturewas cooled on an ice bath
2. stirringThe mixture was stirred for 30 minutes
3. stirringThe resulting mixture was stirred overnight
4. customAfter removal of the solvent, crude residue
5. additionwas taken up with a mixture of ethyl acetate and water
6. filtrationfiltered
7. washorganic layer was washed with 10% hydrochloric acid and saturated sodium bicarbonate solution
8. dry with materialdried over magnesium sulfate
9. customevaporated