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

HRID 419335

반응식

HRID 419335 반응식
[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]

참가 물질

4

반응물 2

HCID 6577Chloroacetyl chlorideHCID 218838753-Methoxy-4-nitrobenzohydrazide

생성물 1

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

시약·촉매·용매 1

HCID 8857Ethyl Acetate용매

실험 절차

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).

후처리

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

출처 및 근거

ORD 기록
ord-745fc27ce7ca455fa04f08fd189a966d
출처 데이터셋
uspto-grants-2012_01
특허 번호
US08093239B2

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