HRID1160345

反应详情

EQUATION

反应方程式

HRID 1160345 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a stirred solution of N—BOC-3-piperidinemethanol (0.50 g, 0.002 mmole) in DCM (10 mL) was added dropwise pyridine (2.42 mL, 0.03 mmole) followed by the addition of methanesulfonyl chloride (0.774 mL, 0.01 mmole). The reaction mixture continued stirring at RT overnight. The reaction mixture was quenched with water. The aqueous layer was extracted with EtOAc (3×5 mL). Combined organic layers were dried over Na2SO4 and concentrated to yield a crude oil, 68, which was used in the next step without further purification. LRMS: 193 (M+-BOC group).

WORKUP

后处理

  1. customThe reaction mixture was quenched with water
  2. extractionThe aqueous layer was extracted with EtOAc (3×5 mL)
  3. dry with materialCombined organic layers were dried over Na2SO4
  4. concentrationconcentrated
  5. customto yield a crude oil, 68, which
  6. customwas used in the next step without further purification