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

HRID 1006347ノート

反応式

HRID 1006347 の反応式
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]

参加物

5

反応物 3

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

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).

後処理

  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

出典と根拠

ORDレコード
ord-a65cfe61ac354c4d84d5166498004d6e
出典データセット
uspto-grants-2004_09
特許番号
US06787543B2

反応ノート

読み込み中…