反应 #1178480

ord-7dfecf5d2f034816a82450775b2ad451

反应方程式

Cl
hydrochloric acid
C[C@@H]1CN(C2CN(C(c3ccccc3)c3ccccc3)C2)C[C@H](C)O1
Cis-4-(1-benzhydryl-3-azetidinyl)-2,6-dimethylmorpholine
C[C@@H]1CN(C2CNC2)C[C@H](C)O1.Cl
title compound
收率 100.0%
C[C@@H]1CN(C2CNC2)C[C@H](C)O1.Cl
Cis-4-(3-azetidinyl)-2,6-dimethylmorpholine hydrochloride
收率 100.0%

溶剂

反应条件

详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    其他The catalyst was removed by filtration
  2. 2
    浓缩the solvent was concentrated under reduced pressure
  3. 3
    workup.ADDITIONA 1N-hydrochloric acid (10 mL) was added to the obtained residue
  4. 4
    洗涤the mixture was washed with diethylether
  5. 5
    浓缩The aqueous layer was concentrated

实验过程

Cis-4-(1-benzhydryl-3-azetidinyl)-2,6-dimethylmorpholine (2.63 g, 7.82 mmol) was dissolved in methanol (40 mL), and 10% palladium hydroxide (wet) (500 mg) and a 1N-hydrochloric acid (5 mL) were added thereto. The mixture was stirred for 24 hours at room temperature under a hydrogen stream at normal pressure. The catalyst was removed by filtration, and the solvent was concentrated under reduced pressure. A 1N-hydrochloric acid (10 mL) was added to the obtained residue, and the mixture was washed with diethylether. The aqueous layer was concentrated to obtain the title compound (1.9 g, 100%) as an amorphous matter.

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US08129366B2uspto-grants-2012_03