Dimethylformamide → 6-chloro-N-(3-fluoropyridin-4-yl)-8-(isoxazol-3-ylamino)imidazo[1,2-b]pyridazine-3-carboxamide

HRID 1943461

反応式

HRID 1943461 の反応式
[O:1]1[CH:5]=[CH:4][C:3]([NH2:6])=[N:2]1.[H-].[Na+].Br[C:10]1[C:11]2[N:12]([C:17]([C:20]([NH:22][C:23]3[CH:28]=[CH:27][N:26]=[CH:25][C:24]=3[F:29])=[O:21])=[CH:18][N:19]=2)[N:13]=[C:14]([Cl:16])[CH:15]=1.CN(C=O)C>C1COCC1>[Cl:16][C:14]1[CH:15]=[C:10]([NH:6][C:3]2[CH:4]=[CH:5][O:1][N:2]=2)[C:11]2[N:12]([C:17]([C:20]([NH:22][C:23]3[CH:28]=[CH:27][N:26]=[CH:25][C:24]=3[F:29])=[O:21])=[CH:18][N:19]=2)[N:13]=1

参加物

6

反応物 4

HCID 6228DimethylformamideHCID 24758Sodium hydrideHCID 18102163-IsoxazolamineHCID 596244958-Bromo-6-chloro-N-(3-fluoropyridin-4-yl)imidazo[1,2-b]pyridazine-3-carboxamide

生成物 1

HCID 596247806-chloro-N-(3-fluoropyridin-4-yl)-8-(isoxazol-3-ylamino)imidazo[1,2-b]pyridazine-3-carboxamide

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

To a solution of isoxazol-3-amine (25.8 mg, 0.307 mmol) in THF (0.5 mL) was added 60% NaH (12.26 mg, 0.307 mmol). The mixture was stirred for 10 min and 5A (40 mg, 0.123 mmol) was added followed by DMF (0.5 mL). The mixture was stirred overnight. The solvent was removed under a stream of nitrogen and water was added. The resulting solid was collected by filtration, rinsed with water, and dried on vacuum to give the title compound as a yellow solid.

後処理

  1. stirringThe mixture was stirred overnight
  2. customThe solvent was removed under a stream of nitrogen and water
  3. additionwas added
  4. filtrationThe resulting solid was collected by filtration
  5. washrinsed with water
  6. customdried on vacuum

出典と根拠

ORDレコード
ord-6d5c087c09914086a7d207d7af4651b6
出典データセット
uspto-grants-2013_03
特許番号
US08389527B2

関連ノート

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