Ethanol → HCID 66733850, 화합물

HRID 2047057노트

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HRID 2047057 반응식
O1[C:5]2([CH2:10][CH2:9][CH:8]([C:11]3[CH:16]=[C:15]([NH2:17])[N:14]4[N:18]=[CH:19][CH:20]=[C:13]4[N:12]=3)[CH2:7][CH2:6]2)[O:4]CC1.CCO.O.O1CCOCC1>C(Cl)Cl>[NH2:17][C:15]1[N:14]2[N:18]=[CH:19][CH:20]=[C:13]2[N:12]=[C:11]([CH:8]2[CH2:7][CH2:6][C:5](=[O:4])[CH2:10][CH2:9]2)[CH:16]=1

참가 물질

6

반응물 4

HCID 702EthanolHCID 962WaterHCID 312751,4-DioxaneHCID 667334895-(1,4-Dioxaspiro[4.5]decan-8-yl)pyrazolo[1,5-a]pyrimidin-7-amine

생성물 1

HCID 66733850HCID 66733850, 화합물수율 93%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

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온도
80 °C

실험 절차

In a 40 mL scintillation vial is combined 5-(1,4-dioxaspiro[4.5]decan-8-yl)pyrazolo[1,5-a]pyrimidin-7-amine (5.54 mmol, 1.52 g), EtOH (10 mL), H2O (4 mL) and 4N HCL:dioxane (4 mL). The vial was capped, sealed and the reaction was heated to 80° C. overnight. After 18 hours, the reaction mixture was cooled to room temperature and diluted with DCM (100 mL). The solution was washed with saturated NaHCO3(aq) and extracted with DCM twice more. The combined organics are dried over Na2SO4 and the solvent removed in vacuo to yield 4-(7-aminopyrazolo[1,5-a]pyrimidin-5-yl)cyclohexanone (1.18 g, 93% yield) as pale orange solid.

후처리

  1. customThe vial was capped
  2. customsealed
  3. temperaturethe reaction mixture was cooled to room temperature
  4. washThe solution was washed with saturated NaHCO3(aq)
  5. extractionextracted with DCM twice more
  6. dry with materialThe combined organics are dried over Na2SO4
  7. customthe solvent removed in vacuo

출처 및 근거

ORD 기록
ord-2f55afef3ace4c72b94aa03ca1522551
출처 데이터셋
uspto-grants-2013_11
특허 번호
US08591943B2

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