HRID267339
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
15 g. (0.052 mole) of Methyl γ-morpholinobutyrate (Cruickshank and Sheehan, J. Am. Chem. Soc. 83, 2891 (1961)) was dissolved in a mixture of 45 ml. of 47% hydrobromic acid and 45 ml. of water and heated for 16 hours at reflux. The solution was taken to dryness under reduced pressure, and the solid which formed was triturated with acetone. The material was filtered and crystallized from 60 ml. of acetic acid to give 12.4 g. (95%) of product as colorless crystals, m.p. 151°-152.5°C. The infrared and nuclear magnetic resonance spectra were consistent with the proposed structure.
WORKUP
后处理
- temperatureat reflux
- customthe solid which formed
- customwas triturated with acetone
- filtrationThe material was filtered
- customcrystallized from 60 ml
- customof acetic acid to give 12.4 g