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

HRID 582054

反応式

HRID 582054 の反応式
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

参加物

3

反応物 2

HCID 785722-ChlorobenzimidazoleHCID 4158521-Benzyl-4-piperidylamine

生成物 1

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

実験手順

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).

後処理

  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

出典と根拠

ORDレコード
ord-d4d8e37fcd0a4bc8977bd503b9a5113f
出典データセット
uspto-grants-1999_07
特許番号
US05922737

関連ノート

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