Hydrochloric Acid → HCID 66733850, 화합물

HRID 1913229노트

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HRID 1913229 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.Cl>C(Cl)Cl.O1CCOCC1>[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

7

반응물 4

HCID 313Hydrochloric AcidHCID 702EthanolHCID 962WaterHCID 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 2

HCID 6344Dichloromethane용매HCID 312751,4-Dioxane용매

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온도
80 °C

실험 절차

In a 40 mL scintillation vial was combined 5-(1,4-dioxaspiro[4.5]decan-8-yl)pyrazolo[1,5-a]pyrimidin-7-amine (Int-5g, 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 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 were dried over Na2SO4 and the solvent was removed in vacuo to yield 4-(7-aminopyrazolo[1,5-a]pyrimidin-5-yl)cyclohexanone (Int-5h) (1.18 g, 93% yield) as a pale orange solid.

후처리

  1. customThe vial was capped
  2. customsealed
  3. temperaturethe reaction 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 were dried over Na2SO4
  7. customthe solvent was removed in vacuo

출처 및 근거

ORD 기록
ord-920a11ede20f46499615c82af0b3ed8f
출처 데이터셋
uspto-grants-2013_12
특허 번호
US08609675B2

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