Water → HCID 85844986、化合物

HRID 1179117ノート

反応式

HRID 1179117 の反応式
[CH3:1][O:2][C:3]1[CH:8]=[CH:7][C:6]([O:9][CH3:10])=[CH:5][C:4]=1[NH:11][C:12]([CH:14]1[CH2:19][CH2:18][CH2:17][CH2:16][CH2:15]1)=O.COC1C=CC(P2(SP(C3C=CC(OC)=CC=3)(=S)S2)=[S:29])=CC=1.O>C1(C)C=CC=CC=1>[CH3:1][O:2][C:3]1[CH:8]=[CH:7][C:6]([O:9][CH3:10])=[CH:5][C:4]=1[NH:11][C:12]([CH:14]1[CH2:19][CH2:18][CH2:17][CH2:16][CH2:15]1)=[S:29]

参加物

5

反応物 3

HCID 962WaterHCID 87949Lawesson's reagentHCID 531821N-(2,5-dimethoxyphenyl)cyclohexanecarboxamide

生成物 1

HCID 85844986HCID 85844986、化合物収率 81.4%

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒

反応条件

温度
100 °C

実験手順

1.46 g (5.54 mmol) of N-(2,5-dimethoxyphenyl)cyclohexanecarboxamide is put into solution in 40 ml of anhydrous toluene. The solution is taken to 100° C., and 3.34 g (8.26 mmol; 1.5 eq.) of Lawesson's reagent are added to the reaction medium which is then maintained under stirring at 100° C. for 4 hours. After returning to ambient temperature, the solution is poured into 50 ml of iced water and extracted using toluene. The organic phases are dried over magnesium sulphate and the solvent is evaporated off. The N-(2,5-dimethoxyphenyl)cyclohexanecarbothioamide is then purified by chromatography on a silica column (eluent: dichloromethane/heptane: 1/1 then 3/2). 1.26 g (yield=81%) of product is obtained in the form of yellow oil.

後処理

  1. customis taken to 100° C.
  2. temperatureis then maintained
  3. customAfter returning to ambient temperature
  4. extractionextracted
  5. dry with materialThe organic phases are dried over magnesium sulphate
  6. customthe solvent is evaporated off
  7. customThe N-(2,5-dimethoxyphenyl)cyclohexanecarbothioamide is then purified by chromatography on a silica column (eluent

出典と根拠

ORDレコード
ord-74144ee1d01748d78edb39e6ff2f4f30
出典データセット
uspto-grants-2007_10
特許番号
US07279467B2

反応ノート

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