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Benzonitrile → HCID 53389671, 화합물

HRID 1020863
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HRID 1020863 반응식
[CH3:1][O:2][C:3](=[O:17])/[CH:4]=[C:5](\[NH:7][C:8]1[CH:13]=[CH:12][C:11]([N+:14]([O-:16])=[O:15])=[CH:10][CH:9]=1)/[CH3:6].[C:18](#[N:25])[C:19]1[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=1>CC([O-])=O.CC([O-])=O.[Cu+2]>[CH3:1][O:2][C:3]([C:4]1[C:18]([C:19]2[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=2)=[N:25][N:7]([C:8]2[CH:13]=[CH:12][C:11]([N+:14]([O-:16])=[O:15])=[CH:10][CH:9]=2)[C:5]=1[CH3:6])=[O:17]
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참가 물질

4

반응물 2

HCID 7505BenzonitrileHCID 5993463HCID 5993463, 화합물

생성물 1

HCID 53389671HCID 53389671, 화합물수율 75%

시약·촉매·용매 1

HCID 8895Cupric acetate촉매

실험 절차

According to AVV A, (Z-3-(4-nitrophenylamino)-but-2-enoic acid methylester (236.2 mg, 1.0 mmol, 1.0 equiv.) was stirred with Cu(OAc)2 (544.9 mg, 3.0 mmol, 3.0 equiv.) into benzonitrile (3.0 ml, 29.4 mmol, 29.4 equiv.) for 14 hours at 120° C. The brown solid obtained as raw product (533.2 mg) was purified by means of column chromatography (silica gel (50 g), CH2Cl2/EtOAc 100:0→90:10→0:100), whereby the pure product was obtained in the form of a slightly yellowish solid (253.5 mg, 0.75 mmol, 75%).

후처리

  1. customThe brown solid obtained as raw product (533.2 mg)
  2. customwas purified by means of column chromatography (silica gel (50 g), CH2Cl2/EtOAc 100:0→90:10→0:100), whereby the pure product

출처 및 근거

ORD 기록
ord-4ae9a98673664c45b31ef4ba9ec0e027
출처 데이터셋
uspto-grants-2014_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08716485B2

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