Ammonia → 1H-benzimidazole-2-carbonitrile

HRID 1033221

반응식

HRID 1033221 반응식
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]

참가 물질

4

반응물 2

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

생성물 1

HCID 8438581H-benzimidazole-2-carbonitrile

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

3.2 Grams of a 2-(trichloromethyl)benzimidazole compound [compound (101)] of the formula (XI) in which X is H and Z is OCF2CFHO was dissolved in 30 ml of ethanol. The resulting solution was added by drops to 4 ml of a 25% aqueous ammonia at 5° C. After stirring for 1 hour at 5° to 15° 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 2.83 g of a 2-cyanobenzimidazole compound [compound (i)] of the formula (II) in which X is H and Z is OCF2CFHO.

후처리

  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

출처 및 근거

ORD 기록
ord-4b31a767e5fe4890bed026a0490f5f0f
출처 데이터셋
uspto-grants-1994_05
특허 번호
US05310747

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