Trifluoroacetic acid → (S)-1'-[3-(3,4-dichloro-phenyl)-4-methylamino-butyl]-[1,4']bipiperidinyl-2-one

HRID 2221073노트

반응식

HRID 2221073 반응식
FC(F)(F)C(O)=O.C(O[C:13](=O)[N:14]([CH2:16][C@H:17]([C:33]1[CH:38]=[CH:37][C:36]([Cl:39])=[C:35]([Cl:40])[CH:34]=1)[CH2:18][CH2:19][N:20]1[CH2:25][CH2:24][CH:23]([N:26]2[CH2:31][CH2:30][CH2:29][CH2:28][C:27]2=[O:32])[CH2:22][CH2:21]1)C)(C)(C)C>ClCCl.[OH-].[Na+]>[Cl:40][C:35]1[CH:34]=[C:33]([C@@H:17]([CH2:16][NH:14][CH3:13])[CH2:18][CH2:19][N:20]2[CH2:21][CH2:22][CH:23]([N:26]3[CH2:31][CH2:30][CH2:29][CH2:28][C:27]3=[O:32])[CH2:24][CH2:25]2)[CH:38]=[CH:37][C:36]=1[Cl:39]

참가 물질

5

반응물 2

HCID 6422Trifluoroacetic acid2회HCID 69224867(S)-[2-(3,4-Dichloro-phenyl)-4-(2-oxo-[1,4']bipiperidinyl-1'-yl)-butyl]-methyl-carbamic acid tert-butyl ester

생성물 1

HCID 69222215(S)-1'-[3-(3,4-dichloro-phenyl)-4-methylamino-butyl]-[1,4']bipiperidinyl-2-one

시약·촉매·용매 2

HCID 6344Dichloromethane용매HCID 14798Sodium Hydroxide용매

실험 절차

Trifluoroacetic acid (13.1 mL) was added to a solution of (S)-[2-(3,4-dichloro-phenyl)-4-(2-oxo-[1,4′]bipiperidinyl-1′-yl)-butyl]-methyl-carbamic acid tert-butyl ester (8.73 g) in dichloromethane (300 mL). After stirring for 30 minutes additional trifluoroacetic acid (13.1 mL) was added. After 1.5 hours the reaction was diluted with aqueous sodium hydroxide, and the layers were separated. The organic layer was washed with water, dried and evacuated to a viscous oil which was not purified further. MS: m/z=412(M+1).

후처리

  1. additionwas added
  2. customthe layers were separated
  3. washThe organic layer was washed with water
  4. customdried
  5. customevacuated to a viscous oil which
  6. customwas not purified further

출처 및 근거

ORD 기록
ord-b7468632f8e049159082dcea7ea0199f
출처 데이터셋
uspto-grants-2008_05
특허 번호
US07368461B2

반응 노트

불러오는 중…