HRID2104313

反应详情

EQUATION

反应方程式

HRID 2104313 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

An 1 N aqueous solution of lithium hydroxide (227 ml, 227 mmol) was added to a solution of 2-oxo-1-azaspiro[3.3]heptane-1-carboxylic acid tert-butylester (48 g, 0.227 mmol) in tetrahydrofuran (200 ml). The reaction mixture was stirred for 2 h. Diethyl ether (200 ml) and water (200 ml) were added. The mixture was stirred for 16 h. The organic layer was isolated. The aqueous phase was extracted with diethyl ether (200 ml). The aqueous phase was acidified with a 10% aqueous solution of sodium hydrogen sulfate until pH 3. The formed precipitation was filtered off, washed with water, and dried in vacuo, to give 38.84 g of (1-(tert-butoxycarbonylamino)cyclobutyl)acetic acid.

WORKUP

后处理

  1. stirringThe mixture was stirred for 16 h
  2. customThe organic layer was isolated
  3. extractionThe aqueous phase was extracted with diethyl ether (200 ml)
  4. customThe formed precipitation
  5. filtrationwas filtered off
  6. washwashed with water
  7. customdried in vacuo