HRID1618782
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
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
- concentrationit was concentrated under reduced pressure
- customPurification by column chromatography (
- washeluting with a gradient of 10-60% EtOAc in hexanes)