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

HRID 1943461

반응식

HRID 1943461 반응식
[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

참가 물질

6

반응물 4

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

생성물 1

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

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-6d5c087c09914086a7d207d7af4651b6
출처 데이터셋
uspto-grants-2013_03
특허 번호
US08389527B2

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