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Sodium Methoxide → tert-Butyl 4-(5-methoxy-pyrazolo[1,5-a]pyrimidin-7-yl)piperazine-1-carboxylate

HRID 333969
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HRID 333969 반응식
Cl[C:2]1[CH:7]=[C:6]([N:8]2[CH2:13][CH2:12][N:11]([C:14]([O:16][C:17]([CH3:20])([CH3:19])[CH3:18])=[O:15])[CH2:10][CH2:9]2)[N:5]2[N:21]=[CH:22][CH:23]=[C:4]2[N:3]=1.[CH3:24][O-:25].[Na+]>CO>[CH3:24][O:25][C:2]1[CH:7]=[C:6]([N:8]2[CH2:13][CH2:12][N:11]([C:14]([O:16][C:17]([CH3:20])([CH3:19])[CH3:18])=[O:15])[CH2:10][CH2:9]2)[N:5]2[N:21]=[CH:22][CH:23]=[C:4]2[N:3]=1
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참가 물질

4

반응물 2

HCID 10942334Sodium MethoxideHCID 86691599tert-Butyl 4-(5-chloro-pyrazolo[1,5-a]pyrimidin-7-yl)piperazine-1-carboxylate

생성물 1

HCID 86691598tert-Butyl 4-(5-methoxy-pyrazolo[1,5-a]pyrimidin-7-yl)piperazine-1-carboxylate수율 98%

시약·촉매·용매 1

HCID 887Methanol용매2회

실험 절차

tert-Butyl 4-(5-chloro-pyrazolo[1,5-a]pyrimidin-7-yl)piperazine-1-carboxylate (1.23 g, 3.65 mmol) was dissolved under an argon atmosphere in anhydrous methanol (6 ml). Sodium methanolat (3.65 ml of a 1M solution in methanol) was added and the mixture was heated under reflux for 9 hours. The solvent was removed under reduced pressure, the residue taken up in dichloromethane, the resulting solution was washed with water, dried over magnesium sulfate, the solvent removed under reduced pressure to yield 1.186 g of a solid (3.56 mmol, 98%). MS (APCI): m/z=334.3 [M+1]+.

후처리

  1. temperaturethe mixture was heated
  2. temperatureunder reflux for 9 hours
  3. customThe solvent was removed under reduced pressure
  4. washthe resulting solution was washed with water
  5. dry with materialdried over magnesium sulfate
  6. customthe solvent removed under reduced pressure

출처 및 근거

ORD 기록
ord-b88dc047dbe140f4920fcce943de36a9
출처 데이터셋
uspto-grants-2014_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08883791B2

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