Ammonia → 1H-benzimidazole-2-carbonitrile

HRID 1033223

反応式

HRID 1033223 の反応式
Cl[C:2](Cl)(Cl)[C:3]1[NH:4][C:5]2[CH:11]=[CH:10][CH:9]=[CH:8][C:6]=2[N:7]=1.[NH3:14]>C(O)C>[C:2]([C:3]1[NH:4][C:5]2[CH:11]=[CH:10][CH:9]=[CH:8][C:6]=2[N:7]=1)#[N:14]

参加物

4

反応物 2

HCID 222AmmoniaHCID 77133Benzimidazole, 2-trichloromethyl-2 回

生成物 1

HCID 8438581H-benzimidazole-2-carbonitrile

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

反応条件

温度
5 °C

実験手順

1.0 Gram of a 2-(trichloromethyl)benzimidazole compound [compound (107)] of the formula (XI) in which X is H and Z is CF2CF2O was dissolved in 20 ml of ethanol. The resulting solution was added by drops to 5 ml of a 25% aqueous ammonia at 5° C. After stirring for 30 minutes at 5° C., the reaction solution was poured into an ice/conc. hydrochloric acid mixture and extracted with ethyl acetate. The organic layer was washed with water and dried over anhydrous sodium sulfate. Removing the solvent from the dried layer by distillation gave 0.6 g of a 2-cyanobenzimidazole compound [compound (vii)] of the formula (II) in which X is H and Z is CF2CF2O.

後処理

  1. extractionhydrochloric acid mixture and extracted with ethyl acetate
  2. washThe organic layer was washed with water
  3. dry with materialdried over anhydrous sodium sulfate
  4. customRemoving the solvent from the dried layer
  5. distillationby distillation

出典と根拠

ORDレコード
ord-9ed2acfd686847febdd259e9d8edfee2
出典データセット
uspto-grants-1994_05
特許番号
US05310747

関連ノート

読み込み中…