Hydrochloric Acid → 3-(5-Ethoxycarbonyl-4-trifluoromethyl-pyrimidin-2-yl)-1-(2-fluorobenzyl)-1H-pyrazolo[3,4-b]pyridine

HRID 351663ノート

反応式

HRID 351663 の反応式
Cl.[F:2][C:3]1[CH:21]=[CH:20][CH:19]=[CH:18][C:4]=1[CH2:5][N:6]1[C:10]2=[N:11][CH:12]=[CH:13][CH:14]=[C:9]2[C:8]([C:15]([NH2:17])=[NH:16])=[N:7]1.Cl.C[O-].[Na+].C(O[CH:29]=[C:30]([C:36](=O)[C:37]([F:40])([F:39])[F:38])[C:31]([O:33][CH2:34][CH3:35])=[O:32])C>CO>[CH2:34]([O:33][C:31]([C:30]1[C:36]([C:37]([F:38])([F:39])[F:40])=[N:16][C:15]([C:8]2[C:9]3[C:10](=[N:11][CH:12]=[CH:13][CH:14]=3)[N:6]([CH2:5][C:4]3[CH:18]=[CH:19][CH:20]=[CH:21][C:3]=3[F:2])[N:7]=2)=[N:17][CH:29]=1)=[O:32])[CH3:35]

参加物

6

反応物 4

HCID 313Hydrochloric AcidHCID 4685753Ethyl 2-(ethoxymethylene)-4,4,4-trifluoro-3-oxobutanoateHCID 10942334Sodium MethoxideHCID 574158441-((2-Fluorophenyl)methyl)-1H-pyrazolo(3,4-b)pyridine-3-carboximidamide hydrochloride

生成物 1

HCID 227142743-(5-Ethoxycarbonyl-4-trifluoromethyl-pyrimidin-2-yl)-1-(2-fluorobenzyl)-1H-pyrazolo[3,4-b]pyridine

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

600 mg of the crude 1-(2-fluorobenzyl)1H-pyrazolo[3,4-b]pyridine-3-carboxamidine hydrochloride (preparable from the amidine 25A by reaction with HCl) are stirred in 30 ml of methanol with 106 mg of sodium methoxide and admixed with 472 mg (1.96 mmol) of ethyl 3-ethoxy-2-trifluoroacetyl-acrylate. The mixture is boiled for 12 hours and the precipitate is then filtered off with suction and washed with ether. This gives 249 mg (27.5% of theory) of crystals.

後処理

  1. filtrationthe precipitate is then filtered off with suction
  2. washwashed with ether

出典と根拠

ORDレコード
ord-1f47298c27af49ccaeec79f5f6e4527f
出典データセット
uspto-grants-2004_06
特許番号
US06743798B1

反応ノート

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