HRID1618782

反应详情

EQUATION

反应方程式

HRID 1618782 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To an ice-cooled solution of tert-butyl 6-bromo-3,3-bis(hydroxymethyl)-2-oxoindoline-1-carboxylate (5.27 g, 14.16 mmol) in DCM (94 mL) was added triethylamine (7.89 mL, 56.6 mmol) followed by methanesulfonyl chloride (2.21 mL, 28.3 mmol). The solution was stirred for 1 h and then it was concentrated under reduced pressure. Purification by column chromatography (eluting with a gradient of 10-60% EtOAc in hexanes) gave tert-butyl 6-bromo-3,3-bis((methylsulfonyloxy)methyl)-2-oxoindoline-1-carboxylate as a white foam. Mass Spectrum (ESI) m/e=550.0 [(M+Na+) (79Br)] and 552.0 [(M+Na+) (81Br)].

WORKUP

后处理

  1. concentrationit was concentrated under reduced pressure
  2. customPurification by column chromatography (
  3. washeluting with a gradient of 10-60% EtOAc in hexanes)