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

HRID 2221073ノート

反応式

HRID 2221073 の反応式
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]

参加物

5

反応物 2

HCID 6422Trifluoroacetic acid2 回HCID 69224867(S)-[2-(3,4-Dichloro-phenyl)-4-(2-oxo-[1,4']bipiperidinyl-1'-yl)-butyl]-methyl-carbamic acid tert-butyl ester

生成物 1

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

試薬・触媒・溶媒 2

HCID 6344Dichloromethane溶媒HCID 14798Sodium Hydroxide溶媒

実験手順

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).

後処理

  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

出典と根拠

ORDレコード
ord-b7468632f8e049159082dcea7ea0199f
出典データセット
uspto-grants-2008_05
特許番号
US07368461B2

反応ノート

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