Potassium Hydroxide → HCID 11482194, 화합물

HRID 890239노트

반응식

HRID 890239 반응식
[Cl:1][C:2]1[CH:3]=[CH:4][CH:5]=[C:6]2[C:10]=1[NH:9][C:8]([CH3:11])=[CH:7]2.[OH-].[K+].Br[CH2:15][CH2:16][CH2:17][S:18][CH3:19]>COCCOCCN(CCOCCOC)CCOCCOC>[Cl:1][C:2]1[CH:3]=[CH:4][CH:5]=[C:6]2[C:10]=1[N:9]([CH2:15][CH2:16][CH2:17][S:18][CH3:19])[C:8]([CH3:11])=[CH:7]2

참가 물질

5

반응물 3

HCID 14797Potassium Hydroxide2회HCID 1144656368731-27-13회HCID 118160627-chloro-2-methyl-1H-indole

생성물 1

HCID 11482194HCID 11482194, 화합물수율 81.4%

시약·촉매·용매 1

HCID 112414Ethanamine, 2-(2-methoxyethoxy)-N,N-bis[2-(2-methoxyethoxy)ethyl]-촉매2회

실험 절차

1.5 g of 7-chloro-2-methyl-1H-indole are mixed with stirring with 1.1 g of ground potassium hydroxide and 0.2 g of TDA-1. The mixture is left stirring for 2 hours at AT, then 3.1 g of 1-bromo-3-methylsulphanylpropane are added dropwise and the mixture is heated at reflux for 24 hours. Ground potassium hydroxide (0.5 g), TDA-1 (0.1 g) and 1.6 g of 1-bromo-3-methylsulphanylpropane are again added. After heating at reflux for 9 hours, 1.6 g of 1-bromo-3-methylsulphanylpropane are again added and the mixture is heated at reflux for 24 hours. The mixture is allowed to return to AT and is then extracted with toluene. The organic phase is washed with a 10% HCl solution, with water and then a saturated NaCl solution. It is dried and evaporated and then the residue is chromatographed on silica while eluting with a cyclohexane/toluene (50/50, v/v) mixture. 1.87 g of the expected compound are obtained.

후처리

  1. waitThe mixture is left
  2. temperaturethe mixture is heated
  3. temperatureat reflux for 24 hours
  4. temperatureAfter heating
  5. temperatureat reflux for 9 hours
  6. temperaturethe mixture is heated
  7. temperatureat reflux for 24 hours
  8. extractionis then extracted with toluene
  9. washThe organic phase is washed with a 10% HCl solution, with water
  10. customIt is dried
  11. customevaporated
  12. customthe residue is chromatographed on silica
  13. washwhile eluting with a cyclohexane/toluene (50/50

출처 및 근거

ORD 기록
ord-c0304803a7114e1bbe60a7f011a9c45a
출처 데이터셋
uspto-grants-2006_02
특허 번호
US06995184B2

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