1-Amino-2-naphthalenethiol → HCID 86642990, 화합물

HRID 1925185

반응식

HRID 1925185 반응식
[NH2:1][C:2]1[C:11]2[C:6](=[CH:7][CH:8]=[CH:9][CH:10]=2)[CH:5]=[CH:4][C:3]=1[SH:12].[CH3:13][C:14]1([C:20](Cl)=[O:21])[CH2:19][CH2:18][CH2:17][CH2:16][CH2:15]1>N1C=CC=CC=1>[CH3:13][C:14]1([C:20]([NH:1][C:2]2[C:11]3[C:6](=[CH:7][CH:8]=[CH:9][CH:10]=3)[CH:5]=[CH:4][C:3]=2[S:12][C:20]([C:14]2([CH3:13])[CH2:19][CH2:18][CH2:17][CH2:16][CH2:15]2)=[O:21])=[O:21])[CH2:19][CH2:18][CH2:17][CH2:16][CH2:15]1

참가 물질

4

반응물 2

HCID 1133141-Amino-2-naphthalenethiolHCID 41892451-Methylcyclohexanecarbonyl chloride

생성물 1

HCID 86642990HCID 86642990, 화합물

시약·촉매·용매 1

HCID 1049Pyridine용매

반응 조건

온도
60 °C

실험 절차

To a solution of 1-amino-naphthalene-2-thiol in pyridine are added two mol equivalents of 1-methyl-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-methyl-cyclohexanecarbothioic acid S-{1-[(1-methyl-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-082f66ab7e2c4045ad8d41ef15b84c89
출처 데이터셋
uspto-grants-2012_05
특허 번호
US08178583B2

연결된 노트

불러오는 중…