Triphenylphosphonium bromide → HCID 24755049、化合物

HRID 268639

反応式

HRID 268639 の反応式
[CH2:1]([NH:8][C:9]([C:11]1[C:15]([CH:16]([CH3:18])[CH3:17])=[C:14]([CH2:19]O)[N:13]([C:21]2[CH:26]=[CH:25][C:24]([F:27])=[CH:23][CH:22]=2)[N:12]=1)=[O:10])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[BrH:28].[C:29]1([P:35]([C:42]2[CH:47]=[CH:46][CH:45]=[CH:44][CH:43]=2)[C:36]2[CH:41]=[CH:40][CH:39]=[CH:38][CH:37]=2)[CH:34]=[CH:33][CH:32]=[CH:31][CH:30]=1>C(#N)C>[Br-:28].[CH2:1]([NH:8][C:9]([C:11]1[C:15]([CH:16]([CH3:18])[CH3:17])=[C:14]([CH2:19][P+:35]([C:36]2[CH:37]=[CH:38][CH:39]=[CH:40][CH:41]=2)([C:42]2[CH:47]=[CH:46][CH:45]=[CH:44][CH:43]=2)[C:29]2[CH:30]=[CH:31][CH:32]=[CH:33][CH:34]=2)[N:13]([C:21]2[CH:26]=[CH:25][C:24]([F:27])=[CH:23][CH:22]=2)[N:12]=1)=[O:10])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1

参加物

4

反応物 2

HCID 80811Triphenylphosphonium bromideHCID 24754975HCID 24754975、化合物

生成物 1

HCID 24755049HCID 24755049、化合物収率 98%

試薬・触媒・溶媒 1

HCID 6342Acetonitrile溶媒

反応条件

温度
80 °C

実験手順

To a solution of 1-(4-fluoro-phenyl)-5-hydroxymethyl-4-isopropyl-1H-pyrazole-3-carboxylic acid benzylamide (0.525 g, 1.43 mmol) in acetonitrile (50 mL) was added triphenylphosphine hydrobromide (0.49 g, 1.43 mmol; commercially available from Sigma Aldrich). The reaction was heated to 80° C. for 24 hr after which time all starting material was consumed as determined by TLC. The reaction solvent was removed under reduced pressure and the resulting white solid was dried under high vacuum for 12 hr to provide [5-benzylcarbamoyl-2-(4-fluoro-phenyl)-4-isopropyl-2H-pyrazol-3-ylmethyl]-triphenyl-phosphonium bromide (0.977 g, 98%) in sufficient purity for use in the next step.

後処理

  1. customwas consumed
  2. customThe reaction solvent was removed under reduced pressure
  3. customthe resulting white solid was dried under high vacuum for 12 hr

出典と根拠

ORDレコード
ord-4cf3b6a1e1594ce88e6d669c3eaa36b9
出典データセット
uspto-grants-2008_11
特許番号
US07446121B2

関連ノート

読み込み中…