1-(2-Ethylbutyl)cyclohexanecarbonyl chloride → HCID 86642989, 화합물

HRID 1925182노트

반응식

HRID 1925182 반응식
[NH2:1][C:2]1[C:3]([SH:12])=[CH:4][C:5]2[C:10]([CH:11]=1)=[CH:9][CH:8]=[CH:7][CH:6]=2.[CH2:13]([CH:15]([CH2:26][CH3:27])[CH2:16][C:17]1([C:23](Cl)=[O:24])[CH2:22][CH2:21][CH2:20][CH2:19][CH2:18]1)[CH3:14]>N1C=CC=CC=1>[CH2:13]([CH:15]([CH2:26][CH3:27])[CH2:16][C:17]1([C:23]([NH:1][C:2]2[C:3]([S:12][C:23]([C:17]3([CH2:16][CH:15]([CH2:26][CH3:27])[CH2:13][CH3:14])[CH2:18][CH2:19][CH2:20][CH2:21][CH2:22]3)=[O:24])=[CH:4][C:5]3[C:10]([CH:11]=2)=[CH:9][CH:8]=[CH:7][CH:6]=3)=[O:24])[CH2:22][CH2:21][CH2:20][CH2:19][CH2:18]1)[CH3:14]

참가 물질

4

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온도
60 °C

실험 절차

To a solution of 3-amino-naphthalene-2-thiol in pyridine are added two mol equivalents of 1-(2-ethyl-butyl)-cyclohexanecarbonyl chloride at room temperature. After completion of the addition, the reaction mixture is heated to 60° C. for 2 hours. The pyridine is then removed under reduced pressure, water is added and the mixture is extracted with ethyl acetate. The combined extracts are washed with sat. NaHCO3-solution, diluted hydrochloric acid and brine, dried (Na2SO4) and concentrated to obtain crude 1-(2-ethyl-butyl)-cyclohexanecarbothioic acid S-(3-{[1-(2-ethyl-butyl)-cyclohexanecarbonyl]-amino}-naphthalen-2-yl)ester.

후처리

  1. additionAfter completion of the addition
  2. customThe pyridine is then removed under reduced pressure, water
  3. additionis added
  4. extractionthe mixture is extracted with ethyl acetate
  5. washThe combined extracts are washed with sat. NaHCO3-solution, diluted hydrochloric acid and brine
  6. dry with materialdried (Na2SO4)
  7. concentrationconcentrated

출처 및 근거

ORD 기록
ord-76691cd0dce34af4b45e9e1322a44b58
출처 데이터셋
uspto-grants-2012_05
특허 번호
US08178583B2

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