2-Bromo-1-(thiophen-3-yl)ethan-1-one → 4-((Bis(3-fluorophenyl)methoxy)carbonyl)-1-methyl-1-(2-oxo-2-(thiophen-3-yl)ethyl)piperidinium bromide

HRID 1910517ノート

反応式

HRID 1910517 の反応式
[Br:1][CH2:2][C:3]([C:5]1[CH:9]=[CH:8][S:7][CH:6]=1)=[O:4].[CH3:10][N:11]1[CH2:16][CH2:15][CH:14]([C:17]([O:19][CH:20]([C:28]2[CH:33]=[CH:32][CH:31]=[C:30]([F:34])[CH:29]=2)[C:21]2[CH:26]=[CH:25][CH:24]=[C:23]([F:27])[CH:22]=2)=[O:18])[CH2:13][CH2:12]1>CCOC(C)=O>[Br-:1].[F:34][C:30]1[CH:29]=[C:28]([CH:20]([C:21]2[CH:26]=[CH:25][CH:24]=[C:23]([F:27])[CH:22]=2)[O:19][C:17]([CH:14]2[CH2:13][CH2:12][N+:11]([CH3:10])([CH2:2][C:3](=[O:4])[C:5]3[CH:9]=[CH:8][S:7][CH:6]=3)[CH2:16][CH2:15]2)=[O:18])[CH:33]=[CH:32][CH:31]=1

参加物

4

反応物 2

HCID 27763792-Bromo-1-(thiophen-3-yl)ethan-1-oneHCID 70925814Bis(3-fluorophenyl)methyl 1-methylpiperidine-4-carboxylate

生成物 1

HCID 866729504-((Bis(3-fluorophenyl)methoxy)carbonyl)-1-methyl-1-(2-oxo-2-(thiophen-3-yl)ethyl)piperidinium bromide収率 54.7%

試薬・触媒・溶媒 1

HCID 8857Ethyl Acetate溶媒

実験手順

2-Bromo-1-(thiophen-3-yl)ethanone (23.7 mg, 0.12 mmol) was added to a solution of bis(3-fluorophenyl)methyl 1-methylpiperidine-4-carboxylate (40 mg, 0.12 mmol, prepared as in example 40) in EtOAc (3 ml). The reaction was stirred at room temperature overnight. The solvent was evaporated, and the crude was purified by preparative HPLC (eluent: CH3CN/H2O) to obtain 4-((bis(3-fluorophenyl)methoxy)carbonyl)-1-methyl-1-(2-oxo-2-(thiophen-3-yl)ethyl)piperidinium bromide (36.1 mg).

後処理

  1. customThe solvent was evaporated
  2. customthe crude was purified by preparative HPLC (eluent: CH3CN/H2O)

出典と根拠

ORDレコード
ord-b024410d0e2e44739b78fe8e56360f5f
出典データセット
uspto-grants-2013_12
特許番号
US08604015B2

反応ノート

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