Ethanol → HCID 67185016, 화합물

HRID 868842노트

반응식

HRID 868842 반응식
[CH3:1][N:2]1[C:10]2[C:5](=[C:6]([CH3:11])[CH:7]=[CH:8][CH:9]=2)[C:4](CC#N)=[CH:3]1.[OH-:15].[K+].[CH2:17]([OH:19])[CH3:18]>O>[CH3:1][N:2]1[C:10]2[C:5](=[C:6]([CH3:11])[CH:7]=[CH:8][CH:9]=2)[C:4]([CH2:18][C:17]([OH:15])=[O:19])=[CH:3]1

참가 물질

5

반응물 3

HCID 702EthanolHCID 14797Potassium HydroxideHCID 67187925HCID 67187925, 화합물

생성물 1

HCID 67185016HCID 67185016, 화합물

시약·촉매·용매 1

HCID 962Water용매2회

실험 절차

(1,4-Dimethyl-1H-indol-3-yl)-acetonitrile (6.0 g, 33 mmol) is suspended in ethanol (150 mL) and then potassium hydroxide (10.6 g, 162 mmol) in water (150 mL) is added to the solution. The reaction is stirred and then heated to reflux for 16 hours. the reaction is then cooled to room temperature and diluted with water. The aqueous layer is washed with DCM (3×150 mL) and then the water layer is cooled to zero and acidified with the addition of 12N HCl. The resulting suspension is extracted with DCM (3×100 mL) and the organic layers are combined, filtered and evaporated in vacuo. The resulting product is used without further purification (3.9 g, 20 mmol, 60%) LC/MS (M++1): 204.7.

후처리

  1. temperatureheated
  2. temperatureto reflux for 16 hours
  3. washThe aqueous layer is washed with DCM (3×150 mL)
  4. temperaturethe water layer is cooled to zero
  5. additionacidified with the addition of 12N HCl
  6. extractionThe resulting suspension is extracted with DCM (3×100 mL)
  7. filtrationfiltered
  8. customevaporated in vacuo
  9. customThe resulting product is used without further purification (3.9 g, 20 mmol, 60%) LC/MS (M++1)

출처 및 근거

ORD 기록
ord-1a5f877132aa4a43b096dd22a1be286e
출처 데이터셋
uspto-grants-2015_03
특허 번호
US08969348B2

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