Water → 1-[2-(4-allyloxy-2-fluoro-benzyloxy)-ethyl]-1H-[1,2,3]triazole

HRID 2113891ノート

反応式

HRID 2113891 の反応式
[H-].[Na+].[CH2:3]([O:6][C:7]1[CH:12]=[CH:11][C:10]([CH2:13]Cl)=[C:9]([F:15])[CH:8]=1)[CH:4]=[CH2:5].[N:16]1([CH2:21][CH2:22][OH:23])[CH:20]=[CH:19][N:18]=[N:17]1.O>CN(C=O)C>[CH2:3]([O:6][C:7]1[CH:12]=[CH:11][C:10]([CH2:13][O:23][CH2:22][CH2:21][N:16]2[CH:20]=[CH:19][N:18]=[N:17]2)=[C:9]([F:15])[CH:8]=1)[CH:4]=[CH2:5]

参加物

6

反応物 4

HCID 962WaterHCID 24758Sodium hydrideHCID 99892372-(1H-1,2,3-triazol-1-yl)ethan-1-olHCID 692933781-Allyloxy-3-fluoro-4-chloromethyl-benzene

生成物 1

HCID 692938261-[2-(4-allyloxy-2-fluoro-benzyloxy)-ethyl]-1H-[1,2,3]triazole収率 103.7%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

816 mg (32.3 mmol) 95% Sodium hydride were given at −50° C. to a solution of 4.32 g (21.5 mmol) 1-allyloxy-3-fluoro-4-chloromethyl-benzene and 2.51 g (22.2 mmol) 2-(1H-[1,2,3]-triazol-1-yl)-ethanol in 30 ml DMF. The mixture was allowed to warm slowly to r.t., stirred overnight and 10 ml water added. The mixture was extracted twice with ethyl acetate, and the combined organic phases dried over Na2SO4. Solvents were removed in vacuum to yield 6.18 g 1-[2-(4-allyloxy-2-fluoro-benzyloxy)-ethyl]-1H-[1,2,3]triazole yellow oil that was used without further purification.

後処理

  1. extractionThe mixture was extracted twice with ethyl acetate
  2. dry with materialthe combined organic phases dried over Na2SO4
  3. customSolvents were removed in vacuum

出典と根拠

ORDレコード
ord-860e3c1e0b61451a8a1cb31e50b10533
出典データセット
uspto-grants-2008_10
特許番号
US07432291B2

反応ノート

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