2-Chlorobenzimidazole → N-(1-Benzylpiperidin-4-yl)-1H-benzimidazol-2-amine

HRID 582054

반응식

HRID 582054 반응식
Cl[C:2]1[NH:6][C:5]2[CH:7]=[CH:8][CH:9]=[CH:10][C:4]=2[N:3]=1.[CH2:11]([N:18]1[CH2:23][CH2:22][CH:21]([NH2:24])[CH2:20][CH2:19]1)[C:12]1[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=1>>[NH:3]1[C:4]2[CH:10]=[CH:9][CH:8]=[CH:7][C:5]=2[N:6]=[C:2]1[NH:24][CH:21]1[CH2:22][CH2:23][N:18]([CH2:11][C:12]2[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=2)[CH2:19][CH2:20]1

참가 물질

3

반응물 2

HCID 785722-ChlorobenzimidazoleHCID 4158521-Benzyl-4-piperidylamine

생성물 1

HCID 16640950N-(1-Benzylpiperidin-4-yl)-1H-benzimidazol-2-amine

실험 절차

Combine 2-chloro-1H-benzimidazole (5.0 g, 33 mmol) and 1-benzyl-4-aminopiperidine (14.2 g, 75 mmol) and heat to about 150° C. After 12 hours, cool and partition between water and chloroform, warming if necessary. Separate the layers and add methanol and toluene to the organic layer. Evaporate the organic layer in vacuo to give a solid. Triturate the solid with ethyl acetate, collect by filtration, and dry to give (1H-benzimidazol-2-yl)(1-benzylpiperidin-4-yl)amine: Rf =0.30 (2% triethylamine/10% methanol/ethyl acetate).

후처리

  1. temperaturecool
  2. custompartition between water and chloroform
  3. temperaturewarming if necessary
  4. customSeparate the layers
  5. additionadd methanol and toluene to the organic layer
  6. customEvaporate the organic layer in vacuo
  7. customto give a solid
  8. customTriturate the solid with ethyl acetate
  9. filtrationcollect by filtration
  10. customdry

출처 및 근거

ORD 기록
ord-d4d8e37fcd0a4bc8977bd503b9a5113f
출처 데이터셋
uspto-grants-1999_07
특허 번호
US05922737

연결된 노트

불러오는 중…