HRID2398885

反应详情

EQUATION

反应方程式

HRID 2398885 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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°. The infrared and nmr spectra are consistent with the proposed structure.

WORKUP

后处理

  1. dissolution83, 2891 (1961) was dissolved in a mixture of 45 ml
  2. temperatureat reflux
  3. customthe solid which formed
  4. customwas triturated with acetone
  5. filtrationThe material was filtered
  6. customcrystallized from 60 ml
  7. customof acetic acid to give 12.4 g