반응식
[Cl:1][C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][C:3]=1[CH2:8][CH2:9][N:10]1[C:15](=[O:16])[C:14]([C:17](OC)=[O:18])=[CH:13][C:12]([C:21]2[CH:26]=[CH:25][C:24]([F:27])=[C:23]([CH3:28])[CH:22]=2)=[N:11]1.O.O.O.O.O.O.[Cl-].[Ce+3].[Cl-].[Cl-].[BH4-].[Na+].[Cl-].[NH4+]>C1COCC1.CO>[Cl:1][C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][C:3]=1[CH2:8][CH2:9][N:10]1[C:15](=[O:16])[C:14]([CH2:17][OH:18])=[CH:13][C:12]([C:21]2[CH:26]=[CH:25][C:24]([F:27])=[C:23]([CH3:28])[CH:22]=2)=[N:11]1참가 물질
반응물 4
생성물 1
시약·촉매·용매 1
실험 절차
To a solution of 2-[2-(2-chlorophenyl)ethyl]-6-(4-fluoro-3-methylphenyl)-4-methoxycarbonyl-2H-pyridazin-3-one (480 mg, 1.20 mmol) in THF/methanol (2 mL/1 mL), cerium(III) chloride hexahydrate (425 mg, 1.20 mmol) was added at −15° C., followed by the addition of sodium borohydride (45 mg, 1.20 mmol). After stirred for 10 minutes, a saturated aqueous solution of ammonium chloride was added to the reaction mixture, and the mixture was extracted with ethyl acetate. The extract was dried over anhydrous sodium sulfate, and was concentrated under reduced pressure. Further, the concentrate was purified by column chromatography on silica gel [hexane/ethyl acetate (2/1)] to yield the title compound as a pale yellow syrupy substance (yield: 11.0%).
후처리
- extractionthe mixture was extracted with ethyl acetate
- dry with materialThe extract was dried over anhydrous sodium sulfate
- concentrationwas concentrated under reduced pressure
- customFurther, the concentrate was purified by column chromatography on silica gel [hexane/ethyl acetate (2/1)]
출처 및 근거
- ORD 기록
- ord-c90e3851495f4d1a8a68fb66a7e26226
- 출처 데이터셋
- uspto-grants-2007_05
- 특허 번호
- US07211577B2
연결된 노트
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