Water → 5-[3-Methyl-4-(4-[1,2,3]triazol-1-yl-butyl)-phenoxymethyl]-2-(4-trifluoromethyl-phenyl)-pyridine

HRID 33484ノート

反応式

HRID 33484 の反応式
[H-].[Na+].[CH3:3][C:4]1[CH:5]=[C:6]([OH:19])[CH:7]=[CH:8][C:9]=1[CH2:10][CH2:11][CH2:12][CH2:13][N:14]1[CH:18]=[CH:17][N:16]=[N:15]1.Cl[CH2:21][C:22]1[CH:23]=[CH:24][C:25]([C:28]2[CH:33]=[CH:32][C:31]([C:34]([F:37])([F:36])[F:35])=[CH:30][CH:29]=2)=[N:26][CH:27]=1.O>CN(C)C=O>[CH3:3][C:4]1[CH:5]=[C:6]([CH:7]=[CH:8][C:9]=1[CH2:10][CH2:11][CH2:12][CH2:13][N:14]1[CH:18]=[CH:17][N:16]=[N:15]1)[O:19][CH2:21][C:22]1[CH:23]=[CH:24][C:25]([C:28]2[CH:29]=[CH:30][C:31]([C:34]([F:37])([F:35])[F:36])=[CH:32][CH:33]=2)=[N:26][CH:27]=1

参加物

6

反応物 4

HCID 962WaterHCID 24758Sodium hydrideHCID 219357755-Chloromethyl-2-(4-trifluoromethyl-phenyl)-pyridineHCID 691096663-Methyl-4-(4-[1,2,3]triazol-1-yl-butyl)phenol

生成物 1

HCID 160650305-[3-Methyl-4-(4-[1,2,3]triazol-1-yl-butyl)-phenoxymethyl]-2-(4-trifluoromethyl-phenyl)-pyridine収率 71%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

反応条件

温度
0 °C

実験手順

15 mg (0.60 mmol) of 95% sodium hydride were added at 0° C. to a solution of 116 mg (0.50 mmol) 3-methyl-4-(4-[1,2,3]triazol-1-yl-butyl)-phenol in 4.0 ml N,N-dimethylformamide and stirred for 30 min. at 0° C. 136 mg (0.50 mmol) 5-chloromethyl-2-(4-trifluoromethyl-phenyl)-pyridine were given to the reaction mixture and stirring continued at r.t overnight. After addition of 8 ml water the mixture was stirred for 1 h, the formed precipitate isolated by filtration, washed with water, methanol/water 1:1, and a small amount of ether to give 165 mg (71%) of the title compound as white powder.

後処理

  1. stirringstirring
  2. customcontinued at r.t overnight
  3. stirringwas stirred for 1 h
  4. customthe formed precipitate isolated by filtration
  5. washwashed with water, methanol/water 1:1

出典と根拠

ORDレコード
ord-0ef35a57c7f94c39bcac5fb99da58734
出典データセット
uspto-grants-2008_09
特許番号
US07429605B2

反応ノート

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