反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
A mixture of dichloromethane (100 mL) and (2-(((4-(1,3-dihydro-1,3-dioxo-2H-isoindol-2-yl)butyl)hydroxyphosphinyl)methyl)-4-phenylbutanoyl)-L-leucine N-phenylamide (2.00 g, 3.17 mmol) from Example 1 was warmed to give a clear solution which was then cooled in an ice bath. Diazomethane (0.3M solution in ether) was added until the yellow color persisted and the solution was stired 10 min longer. Glacial acetic acid (0.080 mL, 84 mg, 1.4 mmol) was added to give a colorless solution which was concentrated under vacuum. Methanol (100 mL) was added and the solution was evaporated again and dried under vacuum to give 2.09 g of crude product which was used in the next reaction without further purification.
WORKUP
后处理
- temperaturewas warmed
- customto give a clear solution which
- temperaturewas then cooled in an ice bath
- customto give a colorless solution which
- concentrationwas concentrated under vacuum
- additionMethanol (100 mL) was added
- customthe solution was evaporated again
- customdried under vacuum