Acetic Anhydride → 1-(4-(3-Methoxy-4-nitrophenyl)piperazin-1-yl)ethanone

HRID 1014210ノート

反応式

HRID 1014210 の反応式
[CH3:1][O:2][C:3]1[CH:4]=[C:5]([N:12]2[CH2:17][CH2:16][NH:15][CH2:14][CH2:13]2)[CH:6]=[CH:7][C:8]=1[N+:9]([O-:11])=[O:10].C(N(CC)CC)C.[C:25](OC(=O)C)(=[O:27])[CH3:26]>ClCCl>[C:25]([N:15]1[CH2:16][CH2:17][N:12]([C:5]2[CH:6]=[CH:7][C:8]([N+:9]([O-:11])=[O:10])=[C:3]([O:2][CH3:1])[CH:4]=2)[CH2:13][CH2:14]1)(=[O:27])[CH3:26]

参加物

5

反応物 3

HCID 7918Acetic AnhydrideHCID 8471TriethylamineHCID 39674091-(3-Methoxy-4-nitrophenyl)piperazine

生成物 1

HCID 594418231-(4-(3-Methoxy-4-nitrophenyl)piperazin-1-yl)ethanone収率 68%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

To a solution of 1-[3-(methyloxy)-4-nitrophenyl]piperazine (0.5 g, 2.11 mmol) and triethylamine (1.27 g, 12.63 mmol, Aldrich) in dichloromethane (25 mL) was added acetic anhydride (0.64 g, 6.35 mmol, Aldrich). After stirring 3 hrs at rt, the reaction was washed with water (25 mL), organic layer adsorbed to silica gel and purified by column chromatography (dichloromethane to 10% methanol/dichloromethane) to give 1-acetyl-4-[3-(methyloxy)-4-nitrophenyl]piperazine (0.4 g, 68%). ESIMS (M+H)+=280.

後処理

  1. washthe reaction was washed with water (25 mL), organic layer
  2. custompurified by column chromatography (dichloromethane to 10% methanol/dichloromethane)

出典と根拠

ORDレコード
ord-374361a6b31346c0afc1b3a287b3180f
出典データセット
uspto-grants-2011_07
特許番号
US07981903B2

反応ノート

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