反应详情

温度

95 °C

To a solution of (2S,4S)-1-cyclohexylmethyl-4-[(1-hydroxy-naphthalene-2-carbonyl)-amino]-pyrrolidine-2-carboxylic acid methyl ester (50 mg) in tetrahydrofuran (7 mL), aq. ammonium hydroxide (15 mL) was added in a seal tube and the mixture was heated for 24 hrs at 95° C. The reaction mixture was concentrated and the aqueous layer was extracted with diethyl ether, washed with brine, dried, concentrated and was purified by column chromatography to obtain (2S,4S)-1-cyclohexylmethyl-4-[(1-hydroxy-naphthalene-2-carbonyl)-amino]-pyrrolidine-2-carboxylic acid amide (8 mg, 16% yield) as a light brown solid. MS calcd. for C23H30N3O3 [(M+H)+] 396, obsd. 396.

1. concentrationThe reaction mixture was concentrated
2. extractionthe aqueous layer was extracted with diethyl ether
3. washwashed with brine
4. customdried
5. concentrationconcentrated
6. customwas purified by column chromatography