Acetic Anhydride → N-{4-[(4-benzhydryl-1-piperidinyl)methyl]phenyl}acetamide

HRID 258823노트

반응식

HRID 258823 반응식
[C:1]1([CH:7]([C:22]2[CH:27]=[CH:26][CH:25]=[CH:24][CH:23]=2)[CH:8]2[CH2:13][CH2:12][N:11]([CH2:14][C:15]3[CH:20]=[CH:19][C:18]([NH2:21])=[CH:17][CH:16]=3)[CH2:10][CH2:9]2)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.[C:28](OC(=O)C)(=[O:30])[CH3:29]>C(O)(=O)C>[C:28]([NH:21][C:18]1[CH:17]=[CH:16][C:15]([CH2:14][N:11]2[CH2:10][CH2:9][CH:8]([CH:7]([C:1]3[CH:2]=[CH:3][CH:4]=[CH:5][CH:6]=3)[C:22]3[CH:23]=[CH:24][CH:25]=[CH:26][CH:27]=3)[CH2:13][CH2:12]2)=[CH:20][CH:19]=1)(=[O:30])[CH3:29]

참가 물질

4

반응물 2

HCID 7918Acetic AnhydrideHCID 202258204-{[4-(Diphenylmethyl)-1-piperidinyl]methyl}benzenamine

생성물 1

HCID 21424837N-{4-[(4-benzhydryl-1-piperidinyl)methyl]phenyl}acetamide

시약·촉매·용매 1

HCID 176Acetic Acid용매

실험 절차

To a solution of 8 parts of 4-{[4-(diphenylmethyl)-1-piperidinyl]methyl}benzenamine in 50 parts of acetic acid is added 5 parts of acetic anhydride. The resultant mixture is heated to the boiling point under reflux and maintained thereat for 10 minutes, then stripped of solvents by vacuum distillation. The residue is combined with 10 volumes of water. The resultant mixture is made alkaline with concentrated ammonium hydroxide. The mixture thus obtained is extracted with dichloromethane. The dichloromethane extract is dried over anhydrous potassium carbonate and then stripped of solvent by vacuum distillation. The residue, recrystallized from benzene, affords N-acetyl-4-{[4-(diphenylmethyl)-1-piperidinyl]methyl}benzenamine melting at approximately 182°-183°. The product has the formula ##STR5##

후처리

  1. temperatureunder reflux
  2. temperaturemaintained
  3. distillationstripped of solvents by vacuum distillation
  4. customThe mixture thus obtained
  5. extractionis extracted with dichloromethane
  6. extractionThe dichloromethane extract
  7. dry with materialis dried over anhydrous potassium carbonate
  8. distillationstripped of solvent by vacuum distillation
  9. customThe residue, recrystallized from benzene

출처 및 근거

ORD 기록
ord-d664fea9c1b846caac6ca05eb08f8072
출처 데이터셋
uspto-grants-1977_07
특허 번호
US04035372

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