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Water → methyl 4-[7-(methylthio)-2H-pyrazolo[4,3-d]pyrimidin-2-yl]benzoate

HRID 1926047
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HRID 1926047 반응식
[CH3:1][S:2][C:3]1[C:4]2[NH:11][N:10]=[CH:9][C:5]=2[N:6]=[CH:7][N:8]=1.F[C:13]1[CH:22]=[CH:21][C:16]([C:17]([O:19][CH3:20])=[O:18])=[CH:15][CH:14]=1.C(=O)([O-])[O-].[K+].[K+].O>CN1CCCC1=O>[CH3:1][S:2][C:3]1[C:4]2[C:5](=[CH:9][N:10]([C:13]3[CH:22]=[CH:21][C:16]([C:17]([O:19][CH3:20])=[O:18])=[CH:15][CH:14]=3)[N:11]=2)[N:6]=[CH:7][N:8]=1
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참가 물질

6

반응물 4

HCID 962WaterHCID 11430Potassium CarbonateHCID 67878Methyl 4-fluorobenzoateHCID 552958947-(methylthio)-1H-pyrazolo[4,3-d]pyrimidine

생성물 1

HCID 67520899methyl 4-[7-(methylthio)-2H-pyrazolo[4,3-d]pyrimidin-2-yl]benzoate수율 49.8%

시약·촉매·용매 1

HCID 13387
N-methyl-2-pyrrolidone
용매

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온도
120 °C

실험 절차

To a solution of 7-(methylthio)-1H-pyrazolo[4,3-d]pyrimidine (100 mg) and methyl 4-fluorobenzoate (102 mg) in 1-methyl-2-pyrrolidone (2 mL) was added potassium carbonate (125 mg), and the mixture was stirred at 120° C. for 3 hrs. After the completion of the reaction, water was added to the reaction mixture and the mixture was stirred at room temperature for 30 min. The resultant solid was collected by filtration, washed with diisopropyl ether and dried to give the title compound (90 mg) as yellow crystals.

후처리

  1. additionwas added to the reaction mixture
  2. stirringthe mixture was stirred at room temperature for 30 min
  3. filtrationThe resultant solid was collected by filtration
  4. washwashed with diisopropyl ether
  5. customdried

출처 및 근거

ORD 기록
ord-59998ee041cc4fae99ae69b4ac05825a
출처 데이터셋
uspto-grants-2012_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08178543B2

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