Potassium Carbonate → (4-(2,6-Difluorobenzyloxy)phenyl)-acetonitrile

HRID 25017

反応式

HRID 25017 の反応式
[OH:1][C:2]1[CH:10]=[CH:9][C:5]([CH2:6][C:7]#[N:8])=[CH:4][CH:3]=1.C([O-])([O-])=O.[K+].[K+].[F:17][C:18]1[CH:25]=[CH:24][CH:23]=[C:22]([F:26])[C:19]=1[CH2:20]Br>CN(C=O)C>[F:17][C:18]1[CH:25]=[CH:24][CH:23]=[C:22]([F:26])[C:19]=1[CH2:20][O:1][C:2]1[CH:10]=[CH:9][C:5]([CH2:6][C:7]#[N:8])=[CH:4][CH:3]=1

参加物

5

反応物 3

HCID 11430Potassium CarbonateHCID 265484-Hydroxybenzyl cyanideHCID 5814352-(Bromomethyl)-1,3-difluorobenzene

生成物 1

HCID 21964471(4-(2,6-Difluorobenzyloxy)phenyl)-acetonitrile

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

To a solution of 4-Hydroxybenzyl cyanide (5 g, 37.5 mmol) and K2CO3 (6.74 g, 48.8 mmol) in dry DMF (20 ml) was added 2,6-Difluorobenzyl bromide (7.77 g, 37.5 mmol). The reaction mixture was stirred for 4 hours at room temperature and concentrated in vacuo. The crude residue was taken in EtOAc and washed with water and brine. The aqueous layer was washed one more time with EtOAc. The combined organic layers were dried over Na2SO4 filtered, and concentrated to provide the title compound as a white solid.

後処理

  1. concentrationconcentrated in vacuo
  2. washwashed with water and brine
  3. washThe aqueous layer was washed one more time with EtOAc
  4. dry with materialThe combined organic layers were dried over Na2SO4
  5. filtrationfiltered
  6. concentrationconcentrated

出典と根拠

ORDレコード
ord-fae8d767f9e949d2abdb4e613181892b
出典データセット
uspto-grants-2005_02
特許番号
US06858602B2

関連ノート

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