反应 #1178476

ord-7a736cebb3d94cfc9ed81b37c1b4d49a

反应方程式

OC1CN(C(c2ccccc2)c2ccccc2)C1
1-Benzhydryl-3-hydroxyazetidine
O=C(O)C(F)(F)F
TFA
O=C(O)C(F)(F)F.OC1CNC1
title compound
收率 99.0%
O=C(O)C(F)(F)F.OC1CNC1
3-Hydroxyazetidine trifluoroacetate
收率 99.0%

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, water (100 mL)
  2. 2
    workup.ADDITIONwas added to the filtrate
  3. 3
    洗涤the mixture was washed three times with ether
  4. 4
    浓缩The aqueous layer was concentrated under reduced pressure

实验过程

1-Benzhydryl-3-hydroxyazetidine (3.0 g, 12.6 mmol) was dissolved in methanol (60 mL), and 10 mL of TFA and 10% palladium hydroxide (1.0 g) were added thereto. The mixture was stirred for 24 hours under a hydrogen stream at normal pressure. The catalyst was removed by filtration, water (100 mL) was added to the filtrate, and the mixture was washed three times with ether. The aqueous layer was concentrated under reduced pressure, and the title compound (2.33 g, 99%) was obtained as an amorphous matter.

来源

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