HRID432235

反应详情

EQUATION

反应方程式

HRID 432235 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of cis 3-((benzyloxy)methyl)-1-cyclobutanol (2.50 g, 0.0130 mol) in pyridine (50 mL) was cooled to 0° C. Methanesulfonyl chloride (1.21 mL, 1.79 g, 0.0126 mol) was added dropwise, keeping the temperature below 2° C. The mixture was stirred for four hours, and then poured into ice water (100 mL) and extracted with ethyl ether (2×50 mL). The combined organic layers were washed with water (3×50 mL) and brine (50 mL). The organic layer was dried over magnesium sulfate and the solvent was removed in vacuo to give cis 3-[(benzyloxy)methyl]cyclobutyl methanesulfonate (2.73 g, 0.0101 mol) as a yellow oil.

WORKUP

后处理

  1. customthe temperature below 2° C
  2. extractionextracted with ethyl ether (2×50 mL)
  3. washThe combined organic layers were washed with water (3×50 mL) and brine (50 mL)
  4. dry with materialThe organic layer was dried over magnesium sulfate
  5. customthe solvent was removed in vacuo