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

HRID 33482
ノート
印刷プレビュー

反応式

HRID 33482 の反応式
[H-].[Na+].[N:3]1([CH2:8][CH2:9][CH2:10][CH2:11][C:12]2[CH:17]=[CH:16][C:15]([OH:18])=[CH:14][CH:13]=2)[CH:7]=[CH:6][N:5]=[N:4]1.Cl[CH2:20][C:21]1[CH:22]=[CH:23][C:24]([C:27]2[CH:32]=[CH:31][C:30]([C:33]([F:36])([F:35])[F:34])=[CH:29][CH:28]=2)=[N:25][CH:26]=1.O>CN(C)C=O>[N:3]1([CH2:8][CH2:9][CH2:10][CH2:11][C:12]2[CH:13]=[CH:14][C:15]([O:18][CH2:20][C:21]3[CH:22]=[CH:23][C:24]([C:27]4[CH:28]=[CH:29][C:30]([C:33]([F:36])([F:34])[F:35])=[CH:31][CH:32]=4)=[N:25][CH:26]=3)=[CH:16][CH:17]=2)[CH:7]=[CH:6][N:5]=[N:4]1
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 962WaterHCID 24758Sodium hydrideHCID 121094944-(4-[1,2,3]Triazol-1-yl-butyl)phenolHCID 219357755-Chloromethyl-2-(4-trifluoromethyl-phenyl)-pyridine

生成物 1

HCID 160650295-[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 6228
Dimethylformamide
溶媒

反応条件

温度
0 °C

実験手順

23 mg (0.90 mmol) of 95% sodium hydride were added at 0° C. to a solution of 163 mg (0.75 mmol) 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. 204 mg (0.75 mmol) 5-chloromethyl-2-(4-trifluoromethyl-phenyl)-pyridine (WO 2005/049573) were given to the reaction mixture and stirring continued at r.t for 2 days. 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. The residue was purified by chromatography on silica (eluent: ethyl acetate) to give 240 mg 71% of the title compound as white powder.

後処理

  1. stirringstirring
  2. waitcontinued at r.t for 2 days
  3. stirringwas stirred for 1 h
  4. customthe formed precipitate isolated by filtration
  5. washwashed with water, methanol/water 1:1
  6. customThe residue was purified by chromatography on silica (eluent: ethyl acetate)

出典と根拠

ORDレコード
ord-89a19ef0ed494e12aaf6cc388993ebae
出典データセット
uspto-grants-2008_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07429605B2

反応ノート

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