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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
ノート
印刷プレビュー

反応式

HRID 1505471 の反応式
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
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 222AmmoniaHCID 24813Phosphorus oxychlorideHCID 178500133HCID 178500133、化合物

生成物 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-one収率 70%

試薬・触媒・溶媒 1

HCID 6342Acetonitrile溶媒

実験手順

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).

後処理

  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

出典と根拠

ORDレコード
ord-ffb5d55c411248968044712179b6d014
出典データセット
uspto-grants-2015_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09216978B2

反応ノート

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