反応 #1985

ord-2fa90453573642919084e8719e36a12a

反応方程式

O=C(O)C1(C(F)(F)F)CCN(Cc2ccccc2)C1
compound
O=C(O)C1(C(F)(F)F)CCN(Cc2ccccc2)C1
1-benzyl-3-trifluoromethylpyrrolidine-3-carboxylic acid
[Al+3].[H-].[H-].[H-].[H-].[Li+]
LAH
OCC1(C(F)(F)F)CCN(Cc2ccccc2)C1
title compound
収率 99.9%
OCC1(C(F)(F)F)CCN(Cc2ccccc2)C1
1-benzyl-3-trifluoromethylpyrrolidine-3-methanol
収率 99.9%

溶媒

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    その他The reaction was quenched by the sequential dropwise addition of 0.35 mL water, 0.35 mL of 15% NaOH and 1.3 mL of water
  2. 2
    workup.STIRRINGthe mixture was stirred for 1 hour
  3. 3
    ろ過filtered
  4. 4
    その他The filtrate was dried
  5. 5
    濃縮concentrated

実験手順

The compound from step 456a (2.32 g) was dissolved in 60 mL of dry THF, 1.12 eq of LAH (1N in dry THF) was added, and the reaction was stirred under N2 for 3 hours. The reaction was quenched by the sequential dropwise addition of 0.35 mL water, 0.35 mL of 15% NaOH and 1.3 mL of water, then the mixture was stirred for 1 hour and filtered. The filtrate was dried and concentrated to give 2.2 g of the title compound.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US05726182uspto-grants-1998_03