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Cyclohexylpropionyl chloride → HCID 68712047, 화합물

HRID 1820128
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HRID 1820128 반응식
[Br:1][C:2]1[CH:7]=[C:6]([N+:8]([O-:10])=[O:9])[CH:5]=[C:4]([C:11]([F:14])([F:13])[F:12])[C:3]=1[NH2:15].[CH:16]1([CH2:22][CH2:23][C:24](Cl)=[O:25])[CH2:21][CH2:20][CH2:19][CH2:18][CH2:17]1>C(#N)C>[Br:1][C:2]1[CH:7]=[C:6]([N+:8]([O-:10])=[O:9])[CH:5]=[C:4]([C:11]([F:14])([F:13])[F:12])[C:3]=1[NH:15][C:24](=[O:25])[CH2:23][CH2:22][CH:16]1[CH2:21][CH2:20][CH2:19][CH2:18][CH2:17]1
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참가 물질

4

반응물 2

HCID 2734098Cyclohexylpropionyl chlorideHCID 114716542-bromo-4-nitro-6-(trifluoromethyl)aniline

생성물 1

HCID 68712047HCID 68712047, 화합물수율 33%

시약·촉매·용매 1

HCID 6342Acetonitrile용매

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온도
150 °C

실험 절차

2-Bromo-4-nitro-6-trifluoromethyl-phenylamine (2.0 g) and cyclohexylpropionyl chloride (1.30 mL) were mixed in acetonitrile (10 mL) and heated to 150° C. for 10 minutes in a sealed microwave process vial. The reaction was cooled to 0° C., the product filtered off and washed with cold acetonitrile (50 mL) affording 0.97 g (33% yield) of the title compound as a yellow solid. The crude product was used without further purification. LC-MS (m/z) 424 (MH+); tR=3.53, (UV, ELSD) 95%, 99%. 1H NMR (500 MHz, DMSO-d6): 0.88 (m, 2H), 1.17 (m, 3H), 1.28 (m, 1H), 1.51 (m, 2H), 1.68 (m, 5H), 2.38 (t, 2H), 8.45 (d, 1H), 8.82 (d, 1H), 10.17 (s, 1H).

후처리

  1. temperatureThe reaction was cooled to 0° C.
  2. filtrationthe product filtered off
  3. washwashed with cold acetonitrile (50 mL)

출처 및 근거

ORD 기록
ord-b71213bd48a7486cbe1c3c592ceaa3e0
출처 데이터셋
uspto-grants-2009_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07601870B2

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