Chloroacetyl chloride → N'-(chloroacetyl)-3-(methyloxy)-4-nitrobenzohydrazide

HRID 419335

反応式

HRID 419335 の反応式
[CH3:1][O:2][C:3]1[CH:4]=[C:5]([CH:10]=[CH:11][C:12]=1[N+:13]([O-:15])=[O:14])[C:6]([NH:8][NH2:9])=[O:7].[Cl:16][CH2:17][C:18](Cl)=[O:19]>CCOC(C)=O>[Cl:16][CH2:17][C:18]([NH:9][NH:8][C:6](=[O:7])[C:5]1[CH:10]=[CH:11][C:12]([N+:13]([O-:15])=[O:14])=[C:3]([O:2][CH3:1])[CH:4]=1)=[O:19]

参加物

4

反応物 2

HCID 6577Chloroacetyl chlorideHCID 218838753-Methoxy-4-nitrobenzohydrazide

生成物 1

HCID 59452892N'-(chloroacetyl)-3-(methyloxy)-4-nitrobenzohydrazide収率 64%

試薬・触媒・溶媒 1

HCID 8857Ethyl Acetate溶媒

実験手順

To 3-(methyloxy)-4-nitrobenzohydrazide (3.65 g, 17.3 mmol) in EtOAc (150 mL) was added chloroacetyl chloride (1.50 mL, 18.8 mmol). The reaction was stirred open to air overnight. The solid was filtered and washed with diethyl ether to provide the title compound (3.17 g, 11.0 mmol, 64%). 1H NMR (400 MHz, DMSO-d6) δ ppm 3.98 (s, 3H), 4.21 (s, 2H), 7.56 (dd, J=8.2, 1.6 Hz, 1H), 7.74 (d, J=1.8 Hz, 1H), 7.99 (d, J=8.1 Hz, 1H), 10.48-10.54 (m, 1H), 10.82 (d, J=1.5 Hz, 1H).

後処理

  1. filtrationThe solid was filtered
  2. washwashed with diethyl ether

出典と根拠

ORDレコード
ord-745fc27ce7ca455fa04f08fd189a966d
出典データセット
uspto-grants-2012_01
特許番号
US08093239B2

関連ノート

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