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llms.txt · MCP 가이드개인정보처리방침 · 이용약관 · 지원v1.8.0
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Ammonia → 3-[5-Fluoro-1-(2,3,6-trifluorobenzyl)-1H-pyrazolo[3,4-b]pyridin-3-yl]-7,7-dimethyl-5,7-dihydro-6H-pyrrolo[2,3-e][1,2,4]triazin-6-one

HRID 1505471
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HRID 1505471 반응식
P(Cl)(Cl)(Cl)=O.[F:6][C:7]1[CH:8]=[C:9]2[C:15]([C:16]3[N:17]=[N:18][C:19]([C:23]([CH3:29])([CH3:28])[C:24]([O:26]C)=O)=[C:20](O)[N:21]=3)=[N:14][N:13]([CH2:30][C:31]3[C:36]([F:37])=[CH:35][CH:34]=[C:33]([F:38])[C:32]=3[F:39])[C:10]2=[N:11][CH:12]=1.[NH3:40]>C(#N)C>[F:6][C:7]1[CH:8]=[C:9]2[C:15]([C:16]3[N:17]=[N:18][C:19]4[C:23]([CH3:29])([CH3:28])[C:24](=[O:26])[NH:40][C:20]=4[N:21]=3)=[N:14][N:13]([CH2:30][C:31]3[C:36]([F:37])=[CH:35][CH:34]=[C:33]([F:38])[C:32]=3[F:39])[C:10]2=[N:11][CH:12]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 222AmmoniaHCID 24813Phosphorus oxychlorideHCID 178500133HCID 178500133, 화합물

생성물 1

HCID 565973473-[5-Fluoro-1-(2,3,6-trifluorobenzyl)-1H-pyrazolo[3,4-b]pyridin-3-yl]-7,7-dimethyl-5,7-dihydro-6H-pyrrolo[2,3-e][1,2,4]triazin-6-one수율 70%

시약·촉매·용매 1

HCID 6342Acetonitrile용매

실험 절차

15 ml of phosphoryl chloride were added to 1.50 g (3.149 mmol) of the compound from Example 82A, and the mixture was stirred overnight. The reaction mixture was then taken up in 222 ml of acetonitrile and, with ice cooling, stirred into 133 ml of concentrated ammonia solution (33% in water). The reaction mixture was stirred at room temperature overnight and then concentrated on a rotary evaporator. Ethanol and water were added to the residue. A precipitate formed, which was filtered off and then washed with diethyl ether. Drying under high vacuum gave 982 mg of the title compound (70% of theory).

후처리

  1. stirringThe reaction mixture was stirred at room temperature overnight
  2. concentrationconcentrated on a rotary evaporator
  3. additionEthanol and water were added to the residue
  4. customA precipitate formed
  5. filtrationwhich was filtered off
  6. washwashed with diethyl ether
  7. customDrying under high vacuum

출처 및 근거

ORD 기록
ord-ffb5d55c411248968044712179b6d014
출처 데이터셋
uspto-grants-2015_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09216978B2

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