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

HRID 2113891노트

반응식

HRID 2113891 반응식
[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]

참가 물질

6

반응물 4

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

생성물 1

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

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-860e3c1e0b61451a8a1cb31e50b10533
출처 데이터셋
uspto-grants-2008_10
특허 번호
US07432291B2

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