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Water → 2-Methyl-3-[4-(4-[1,2,3]triazol-1-yl-butyl)-phenoxymethyl]-6-(4-trifluoromethoxy-phenyl)-pyridine

HRID 33496
ノート
印刷プレビュー

反応式

HRID 33496 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[C:22]([CH3:38])=[N:23][C:24]([C:27]2[CH:32]=[CH:31][C:30]([O:33][C:34]([F:37])([F:36])[F:35])=[CH:29][CH:28]=2)=[CH:25][CH:26]=1.O>CN(C)C=O>[CH3:38][C:22]1[C:21]([CH2:20][O:18][C:15]2[CH:14]=[CH:13][C:12]([CH2:11][CH2:10][CH2:9][CH2:8][N:3]3[CH:7]=[CH:6][N:5]=[N:4]3)=[CH:17][CH:16]=2)=[CH:26][CH:25]=[C:24]([C:27]2[CH:28]=[CH:29][C:30]([O:33][C:34]([F:36])([F:37])[F:35])=[CH:31][CH:32]=2)[N:23]=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 219357213-Chloromethyl-2-methyl-6-(4-trifluoromethoxy-phenyl)-pyridine

生成物 1

HCID 160653002-Methyl-3-[4-(4-[1,2,3]triazol-1-yl-butyl)-phenoxymethyl]-6-(4-trifluoromethoxy-phenyl)-pyridine収率 50.3%

試薬・触媒・溶媒 1

HCID 6228
Dimethylformamide
溶媒

反応条件

温度
0 °C

実験手順

17 mg (0.42 mmol) of 60% sodium hydride were added to at 0° C. to a solution of 91 mg (0.42 mmol) 4-(4-[1,2,3]triazol-1-yl-butyl)-phenol in 6.0 ml N,N-dimethylformamide and stirred for 30 min. at 0° C. 127 mg (0.42 mmol) 3-chloromethyl-2-methyl-6-(4-trifluoromethoxy-phenyl)-pyridine (WO 2005/049573) were given to the reaction mixture and stirring continued at room temperature (r.t.) overnight. After addition of 12 ml water the mixture was stirred for 1 h, the formed precipitate isolated by filtration, washed with water, n-heptane, and ether. The residue was dried at 40° C. in vacuum to give 102 mg (50%) of the title compound as white powder.

後処理

  1. stirringstirring
  2. customcontinued at room temperature
  3. custom(r.t.) overnight
  4. stirringwas stirred for 1 h
  5. customthe formed precipitate isolated by filtration
  6. washwashed with water, n-heptane, and ether
  7. customThe residue was dried at 40° C. in vacuum

出典と根拠

ORDレコード
ord-70e7f5f3f87e42d6b5d00bee7e6b0a88
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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