Water → HCID 85844986, 화합물

HRID 1179117노트

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HRID 1179117 반응식
[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]

참가 물질

5

반응물 3

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

생성물 1

HCID 85844986HCID 85844986, 화합물수율 81.4%

시약·촉매·용매 1

HCID 1140Toluene용매

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온도
100 °C

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-74144ee1d01748d78edb39e6ff2f4f30
출처 데이터셋
uspto-grants-2007_10
특허 번호
US07279467B2

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