Water → 3-(3-Fluoro-phenyl)-6-methoxy-1H-indazole-5-carbonitrile

HRID 503157ノート

反応式

HRID 503157 の反応式
F[C:2]1[C:9]([C:10](=O)[C:11]2[CH:16]=[CH:15][CH:14]=[C:13]([F:17])[CH:12]=2)=[CH:8][C:5]([C:6]#[N:7])=[C:4]([O:19][CH3:20])[CH:3]=1.O.[NH2:22][NH2:23].O>O1CCCC1.CO>[F:17][C:13]1[CH:12]=[C:11]([C:10]2[C:9]3[C:2](=[CH:3][C:4]([O:19][CH3:20])=[C:5]([C:6]#[N:7])[CH:8]=3)[NH:23][N:22]=2)[CH:16]=[CH:15][CH:14]=1

参加物

6

反応物 3

HCID 962WaterHCID 24654Hydrazine hydrate (1:1)HCID 222610354-Fluoro-5-(3-fluoro-benzoyl)-2-methoxy-benzonitrile

生成物 1

HCID 222607803-(3-Fluoro-phenyl)-6-methoxy-1H-indazole-5-carbonitrile

試薬・触媒・溶媒 2

HCID 887Methanol溶媒HCID 8028Tetrahydrofuran溶媒

実験手順

A total of 203 mg of 4-fluoro-5-(3-fluoro-benzoyl)-2-methoxy-benzonitrile obtained in Production Example II-1-c was dissolved in 3 ml of tetrahydrofuran and 3 ml of methanol, 7.4 ml of hydrazine monohydrate was added at room temperature under stirring, and the mixture was stirred at room temperature for 14 hours. Then, water was added and the mixture was extracted with ethyl acetate. The resulting organic layer was washed with 1 N hydrochloric acid, saturated aqueous sodium hydrogencarbonate solution and brine, dried over magnesium sulfate and the solvent was evaporated. The resulting crystals were washed with diethyl ether, to give 172 mg of the title compound as pale yellow crystals.

後処理

  1. stirringthe mixture was stirred at room temperature for 14 hours
  2. extractionthe mixture was extracted with ethyl acetate
  3. washThe resulting organic layer was washed with 1 N hydrochloric acid, saturated aqueous sodium hydrogencarbonate solution and brine
  4. dry with materialdried over magnesium sulfate
  5. customthe solvent was evaporated
  6. washThe resulting crystals were washed with diethyl ether

出典と根拠

ORDレコード
ord-7b01830d492b4a1b800c43e578609885
出典データセット
uspto-grants-2010_08
特許番号
US07776890B2

反応ノート

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