Hydrochloric Acid → 1-{3-[4-(diphenylmethyl)piperazinyl]propyl}-1H-benzimidazol-2-amine

HRID 2050317노트

반응식

HRID 2050317 반응식
COC(=O)[NH:4][C:5]1[N:9]([CH2:10][CH2:11][CH2:12][N:13]2[CH2:18][CH2:17][N:16]([CH:19]([C:26]3[CH:31]=[CH:30][CH:29]=[CH:28][CH:27]=3)[C:20]3[CH:25]=[CH:24][CH:23]=[CH:22][CH:21]=3)[CH2:15][CH2:14]2)[C:8]2[CH:32]=[CH:33][CH:34]=[CH:35][C:7]=2[N:6]=1.Cl>C(O)C>[C:26]1([CH:19]([C:20]2[CH:25]=[CH:24][CH:23]=[CH:22][CH:21]=2)[N:16]2[CH2:17][CH2:18][N:13]([CH2:12][CH2:11][CH2:10][N:9]3[C:8]4[CH:32]=[CH:33][CH:34]=[CH:35][C:7]=4[N:6]=[C:5]3[NH2:4])[CH2:14][CH2:15]2)[CH:27]=[CH:28][CH:29]=[CH:30][CH:31]=1

참가 물질

4

반응물 2

HCID 313Hydrochloric AcidHCID 13105584methyl [1-{3-[4-(diphenylmethyl)-1-piperazinyl]propyl}-1H-benzimidazol-2-yl]carbamate

생성물 1

HCID 131055851-{3-[4-(diphenylmethyl)piperazinyl]propyl}-1H-benzimidazol-2-amine

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

A mixture of 12 parts of methyl[1-{3-[4-(diphenylmethyl)-1-piperazinyl]-propyl}-1H-benzimidazol-2-yl]carbamate, 60 parts of a concentrated hydrochloric acid solution and 80 parts of ethanol is stirred and refluxed overnight. The reaction mixture is evaporated and water is added to the residue. The free base is liberated in the conventional manner with ammonium hydroxide and extracted with trichloromethane. The extract is dried, filtered and evaporated. The residue is crystallized from ethanol. The product is filtered off and dried, yielding 1-{3-[4-(diphenylmethyl)-1-piperazinyl]propyl}-1H-benzimidazol-2-amine; mp. 228.7° C.

후처리

  1. temperaturerefluxed overnight
  2. customThe reaction mixture is evaporated
  3. additionwater is added to the residue
  4. extractionextracted with trichloromethane
  5. customThe extract is dried
  6. filtrationfiltered
  7. customevaporated
  8. customThe residue is crystallized from ethanol
  9. filtrationThe product is filtered off
  10. customdried

출처 및 근거

ORD 기록
ord-6aada3fcf4964279a95b7baf93827ba0
출처 데이터셋
uspto-grants-1980_04
특허 번호
US04200641

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