HRID1489791

反应详情

EQUATION

反应方程式

HRID 1489791 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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

  1. temperaturewas warmed
  2. customto give a clear solution which
  3. temperaturewas then cooled in an ice bath
  4. customto give a colorless solution which
  5. concentrationwas concentrated under vacuum
  6. additionMethanol (100 mL) was added
  7. customthe solution was evaporated again
  8. customdried under vacuum