반응식
Br[C:2]1[CH:3]=[N:4][N:5]([CH2:10][C:11]([NH:13][CH2:14][C:15]2[CH:20]=[CH:19][N:18]=[CH:17][CH:16]=2)=[O:12])[C:6](=[O:9])[C:7]=1[Br:8].[CH3:21][CH:22]1[CH:30]([OH:31])[CH2:29][CH:25]2[C:26]([CH3:28])([CH3:27])[CH:23]1[CH2:24]2.[H-].[Na+].O>O1CCOCC1>[Br:8][C:7]1[C:6](=[O:9])[N:5]([CH2:10][C:11]([NH:13][CH2:14][C:15]2[CH:20]=[CH:19][N:18]=[CH:17][CH:16]=2)=[O:12])[N:4]=[CH:3][C:2]=1[O:31][C@@H:30]1[CH2:29][C@@H:25]2[CH2:24][C@@H:23]([C:26]2([CH3:28])[CH3:27])[C@H:22]1[CH3:21]참가 물질
6
반응물 4
생성물 1
시약·촉매·용매 1
반응 조건
- 온도
- 100 °C
실험 절차
To 2-(4,5-dibromo-6-oxopyridazin-1(6H)-yl)-N-(pyridin-4-ylmethyl)acetamide (50 mg, 0.124 mmol) and (1R,2R,3R,5S)-(−)-isopinocampheol (50 mg, 0.324 mmol) in 1,4-dioxane (2 mL), sodium hydride (15 mg, 0.313 mmol) was added at 0° C., and stirred at 100° C. for 5 days. After completion of the reaction, the reaction mixture was mixed with water and extracted with chloroform and ethyl acetate. The combined organic layer was evaporated under reduced pressure. The resulting residue was purified by silica gel column chromatography (ethyl acetate) to give the desired product (1.7 mg, 3% yield).
후처리
- customAfter completion of the reaction
- extractionextracted with chloroform and ethyl acetate
- customThe combined organic layer was evaporated under reduced pressure
- customThe resulting residue was purified by silica gel column chromatography (ethyl acetate)
출처 및 근거
- ORD 기록
- ord-c56953d6b35a44e2a5f9e7b82d1c8e60
- 출처 데이터셋
- uspto-grants-2013_05
- 특허 번호
- US08440666B2
연결된 노트
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