Hydrochloric Acid → HCID 178437869, 화합물

HRID 1600811노트

반응식

HRID 1600811 반응식
[Na].[CH:2]1([N:7]2[C:11]([NH2:12])=[C:10]([C:13]([NH2:15])=[O:14])[C:9]([CH2:16][CH3:17])=[N:8]2)[CH2:6][CH2:5][CH2:4][CH2:3]1.[F:18][C:19]([F:33])([F:32])[C:20]1[CH:25]=[CH:24][C:23]([CH2:26][C:27](OCC)=O)=[CH:22][CH:21]=1.Cl>C(O)C.O>[CH:2]1([N:7]2[C:11]3=[N:12][C:27]([CH2:26][C:23]4[CH:22]=[CH:21][C:20]([C:19]([F:18])([F:32])[F:33])=[CH:25][CH:24]=4)=[N:15][C:13](=[O:14])[C:10]3=[C:9]([CH2:16][CH3:17])[NH:8]2)[CH2:3][CH2:4][CH2:5][CH2:6]1

참가 물질

7

반응물 4

HCID 313Hydrochloric AcidHCID 5360545SodiumHCID 14134124Ethyl (4-(trifluoromethyl)phenyl)acetateHCID 224493525-amino-1-cyclopentyl-3-ethyl-1H-pyrazole-4-carboxamide

생성물 1

HCID 178437869HCID 178437869, 화합물수율 57.5%

시약·촉매·용매 2

HCID 702Ethanol용매HCID 962Water용매

실험 절차

Sodium (622 mg) was dissolved in ethanol (45 mL) and then 1-cyclopentyl-3-ethyl-5-amino-1H-pyrazole-4-carboxamide (3.0 g, 13.5 mmol), followed by ethyl 4-trifluoromethylphenylacetate (6.27 g, 27 mmol) were added. The reaction mixture was refluxed overnight, cooled to room temperature, and the solvent was stripped. Water, followed by 2N HCl were added to the residue and the product was collected by filtration, recrystallized from ether and dried at 110° C. and 0.2 mm Hg to afford 3.03 g of 1-cyclopentyl-3-ethyl-6-(4-trifluoromethylphenylmethyl)pyrazolo[3,4-d]pyrimidin-4-one, m.p. 212-213° C.

후처리

  1. additionwere added
  2. temperatureThe reaction mixture was refluxed overnight
  3. additionwere added to the residue
  4. filtrationthe product was collected by filtration
  5. customrecrystallized from ether
  6. customdried at 110° C.

출처 및 근거

ORD 기록
ord-aecf132789cb46b39c61f67741bb4186
출처 데이터셋
uspto-grants-1999_11
특허 번호
US05977118

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