1-Amino-2-naphthalenethiol → HCID 86642990、化合物

HRID 1925185

反応式

HRID 1925185 の反応式
[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

参加物

4

反応物 2

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

生成物 1

HCID 86642990HCID 86642990、化合物

試薬・触媒・溶媒 1

HCID 1049Pyridine溶媒

反応条件

温度
60 °C

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-082f66ab7e2c4045ad8d41ef15b84c89
出典データセット
uspto-grants-2012_05
特許番号
US08178583B2

関連ノート

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