HRID1051014
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
产物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
Methyl 1-(methylcarbamoyl)cyclopropanecarboxylate 5b (942 mg, 6 mmol) was dissolved in 10 mL of tetrahydrofuran in a dry ice-acetone bath, by addition of a solution of diisobutylaluminum hydride in tetrahydrofuran (1 M, 18 mL), then the reaction solution was stirred for 1 h, followed by addition of 3 mL of water. After removing the dry ice-acetone bath, the reaction solution was continuously stirred at room temperature for 1 h. The reaction solution was filtered, and the filtrate was concentrated under reduced pressure to obtain the title product 1-(hydroxymethyl)-N-methyl cyclopropanecarboxamide 5c (800 mg, a yellow solid), which was used directly in the next step.
WORKUP
后处理
- customAfter removing the dry ice-acetone bath
- stirringthe reaction solution was continuously stirred at room temperature for 1 h
- filtrationThe reaction solution was filtered
- concentrationthe filtrate was concentrated under reduced pressure