Water → 6-(2-Fluoro-4-trifluoromethyl-phenyl)-2-methyl-3-[3-methyl-4-(4-[1,2,3]triazol-1-yl-butyl)-phenoxymethyl]-pyridine

HRID 33546ノート

反応式

HRID 33546 の反応式
[CH3:1][C:2]1[CH:3]=[C:4]([OH:17])[CH:5]=[CH:6][C:7]=1[CH2:8][CH2:9][CH2:10][CH2:11][N:12]1[CH:16]=[CH:15][N:14]=[N:13]1.[H-].[Na+].Cl[CH2:21][C:22]1[C:23]([CH3:39])=[N:24][C:25]([C:28]2[CH:33]=[CH:32][C:31]([C:34]([F:37])([F:36])[F:35])=[CH:30][C:29]=2[F:38])=[CH:26][CH:27]=1.O>CN(C)C=O>[F:38][C:29]1[CH:30]=[C:31]([C:34]([F:36])([F:37])[F:35])[CH:32]=[CH:33][C:28]=1[C:25]1[N:24]=[C:23]([CH3:39])[C:22]([CH2:21][O:17][C:4]2[CH:5]=[CH:6][C:7]([CH2:8][CH2:9][CH2:10][CH2:11][N:12]3[CH:16]=[CH:15][N:14]=[N:13]3)=[C:2]([CH3:1])[CH:3]=2)=[CH:27][CH:26]=1

参加物

6

反応物 4

HCID 962WaterHCID 24758Sodium hydrideHCID 69106508HCID 69106508、化合物HCID 691096663-Methyl-4-(4-[1,2,3]triazol-1-yl-butyl)phenol

生成物 1

HCID 160653046-(2-Fluoro-4-trifluoromethyl-phenyl)-2-methyl-3-[3-methyl-4-(4-[1,2,3]triazol-1-yl-butyl)-phenoxymethyl]-pyridine収率 76%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

反応条件

温度
0 °C

実験手順

A solution of 153 mg (0.66 mmol) 3-methyl-4-(4-[1,2,3]triazol-1-yl-butyl)phenol in 8.0 ml N,N-dimethylformamide was treated at 0° C. with 26 mg (0.66 mmol) of 60% sodium hydride and stirred at 0° C. for 30 min. Then 200 mg (0.66 mmol) 3-Chloromethyl-6-(2-fluoro-4-trifluoromethyl-phenyl)-2-methyl-pyridine were added and stirred continued at r. t. over night. After addition of 16 ml water, the precipitate was isolated, washed thoroughly with water and diisopropylether. The residue was dried at 40° C. to give 250 mg (76%) of the title compound as light brown powder.

後処理

  1. stirringstirred
  2. waitover night
  3. customthe precipitate was isolated
  4. washwashed thoroughly with water and diisopropylether
  5. customThe residue was dried at 40° C.

出典と根拠

ORDレコード
ord-14cd45f37c694cc88052a057ffa1e8b9
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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