HRID1185432

反应详情

EQUATION

反应方程式

HRID 1185432 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To 100 ml of a saturated solution of hydrochloric acid in ethanol 5 g of 4-[(S)-4-tert-Butoxycarbonyl-2-({4-[2-((S)-2-cyclobutylcarbamoyl-pyrrolidin-1-yl)-2-oxo-ethoxy]-7-methyl-quinoline-2-carbonyl}-amino)-butyryl]-piperazine-1-carboxylic acid ethyl ester was added and the mixture was stirred for 2 h. Then, 30 ml of toluene was added and the solvents were removed under reduced pressure. The residue was filtered through a plug of silica gel eluting with a gradient of n-heptane/ethyl acetate. The fractions containing the product were combined and the solvent evaporated under reduced pressure. The residue was purified by re-crystallisation from n-heptane/ethyl acetate and dried under reduced pressure. Yield: 3.8 g MS (ES+): m/e=709.

WORKUP

后处理

  1. customthe solvents were removed under reduced pressure
  2. filtrationThe residue was filtered through a plug of silica gel eluting with a gradient of n-heptane/ethyl acetate
  3. additionThe fractions containing the product
  4. customthe solvent evaporated under reduced pressure
  5. customThe residue was purified by re-crystallisation from n-heptane/ethyl acetate
  6. customdried under reduced pressure