N-Bromophthalimide → 1-[3-(bromomethyl)-4-fluorophenyl]-5-(trifluoromethyl)-1H-tetrazole

HRID 1006347노트

반응식

HRID 1006347 반응식
N(C(C)(CC(OC)(C)C)C#N)=NC(C)(CC(C)(OC)C)C#N.[F:23][C:24]1[CH:29]=[CH:28][C:27]([N:30]2[C:34]([C:35]([F:38])([F:37])[F:36])=[N:33][N:32]=[N:31]2)=[CH:26][C:25]=1[CH3:39].[Br:40]N1C(=O)C2=CC=CC=C2C1=O>ClCCl>[Br:40][CH2:39][C:25]1[CH:26]=[C:27]([N:30]2[C:34]([C:35]([F:38])([F:36])[F:37])=[N:33][N:32]=[N:31]2)[CH:28]=[CH:29][C:24]=1[F:23]

참가 물질

5

반응물 3

HCID 75542N-BromophthalimideHCID 858672,2'-Azobis(2,4-dimethyl-4-methoxyvaleronitrile)HCID 226746621-(4-fluoro-3-methylphenyl)-5-(trifluoromethyl)-1H-tetrazole

생성물 1

HCID 226746671-[3-(bromomethyl)-4-fluorophenyl]-5-(trifluoromethyl)-1H-tetrazole

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

2,2′-Azobis(4-methoxy-2,4-dimethylvaleronitrile) (50 mg) was added by three portions to the mixture of 1-(4-fluoro-3-methylphenyl)-5-(trifluoromethyl)-1H-tetrazole and N-bromophtalimide (1.44 g) in dichloromethane (16 ml) at 30° C. and the whole was stirred at reflux for 3 hours. After being cooled to room temperature, the mixture was washed with aqueous sodium hydrogen carbonate and aqueous sodium thiosulfate successively. The organic layer was separated, dried over magnesium sulfate, and evaporated under reduced pressure to give a crude 1-[3-(bromomethyl)-4-fluorophenyl]-5-(trifluoromethyl)-1H-tetrazole (3:7).

후처리

  1. temperatureat reflux for 3 hours
  2. washthe mixture was washed with aqueous sodium hydrogen carbonate and aqueous sodium thiosulfate successively
  3. customThe organic layer was separated
  4. dry with materialdried over magnesium sulfate
  5. customevaporated under reduced pressure

출처 및 근거

ORD 기록
ord-a65cfe61ac354c4d84d5166498004d6e
출처 데이터셋
uspto-grants-2004_09
특허 번호
US06787543B2

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