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2-Chloro-6-methyl-4-nitroaniline → HCID 67406977, 화합물

HRID 1158684
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인쇄 미리보기

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HRID 1158684 반응식
[Cl:1][C:2]1[CH:7]=[C:6]([N+:8]([O-:10])=[O:9])[CH:5]=[C:4]([CH3:11])[C:3]=1[NH2:12].[CH:13]1([CH2:18][C:19](Cl)=[O:20])[CH2:17][CH2:16][CH2:15][CH2:14]1>C(#N)C>[Cl:1][C:2]1[CH:7]=[C:6]([N+:8]([O-:10])=[O:9])[CH:5]=[C:4]([CH3:11])[C:3]=1[NH:12][C:19](=[O:20])[CH2:18][CH:13]1[CH2:17][CH2:16][CH2:15][CH2:14]1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 27334602-Chloro-6-methyl-4-nitroanilineHCID 3485182Cyclopentylacetyl chloride

생성물 1

HCID 67406977HCID 67406977, 화합물수율 58%

시약·촉매·용매 1

HCID 6342Acetonitrile용매

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온도
150 °C

실험 절차

2-Chloro-6-methyl-4-nitro-phenylamine (6.0 g) and cyclopentylacetyl chloride (5.1 g) were dissolved in acetonitrile (45 mL) and heated to 150° C. for 20 minutes in a sealed microwave process vessel. The reaction mixture was cooled to 0° C. and the precipitated product collected by filtration and washed with cold acetonitrile to furnish 5.5 g (58%) of the title compound as a yellow solid. 1H NMR (500 MHz, DMSO-d6): 1.24 (m, 2H), 1.58 (m, 4H), 1.78 (m, 2H), 2.27 (m, 1H), 2.30 (s, 3H), 2.38 (d, 2H), 8.15 (d, 1H), 8.18 (d, 1H), 9.83 (s, 1H).

후처리

  1. temperatureThe reaction mixture was cooled to 0° C.
  2. filtrationthe precipitated product collected by filtration
  3. washwashed with cold acetonitrile

출처 및 근거

ORD 기록
ord-e1430360556f434abaa0856ac1978a05
출처 데이터셋
uspto-grants-2010_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07812023B2

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