반응식
[H-].[Na+].[C:3]([N:6]1[C:14]2[C:9](=[CH:10][CH:11]=[C:12]([N:15]3[C:19](=[O:20])[C:18]([CH3:22])([CH3:21])[NH:17][C:16]3=[O:23])[CH:13]=2)[C:8]([CH3:25])([CH3:24])[CH2:7]1)(=[O:5])[CH3:4].[Cl:26][C:27]1[CH:32]=[C:31]([CH2:33]Cl)[CH:30]=[CH:29][N:28]=1>CN(C)C=O.O>[C:3]([N:6]1[C:14]2[C:9](=[CH:10][CH:11]=[C:12]([N:15]3[C:19](=[O:20])[C:18]([CH3:22])([CH3:21])[N:17]([CH2:33][C:31]4[CH:30]=[CH:29][N:28]=[C:27]([Cl:26])[CH:32]=4)[C:16]3=[O:23])[CH:13]=2)[C:8]([CH3:25])([CH3:24])[CH2:7]1)(=[O:5])[CH3:4]참가 물질
반응물 3
생성물 1
시약·촉매·용매 2
반응 조건
- 온도
- 25 °C
실험 절차
To 949 mg of sodium hydride are added dropwise, under argon, 5 mL of dimethylformamide, followed by addition of a solution of 6.8 g of 3-(1-acetyl-3,3-dimethyl-2,3-dihydro-1H-indol-6-yl)-5,5-dimethylimidazolidine-2,4-dione obtained in stage g) below in 40 mL of dimethylformamide. The solution obtained is stirred for 1.5 hours at 25° C., followed by addition of 5.24 g of 2-chloro-4-chloromethylpyridine obtained in stage b) below. The reaction mixture is stirred at room temperature for 15 hours and diluted with 300 mL of water, and the solid formed is filtered off, washed with three times 20 mL of water and with twice 20 mL of diethyl ether and dried to give 8.8 g of 3-(1-acetyl-3,3-dimethyl-2,3-dihydro-1H-indol-6-yl)-1-[(2-chloropyridin-4-yl)methyl]-5,5-dimethylimidazolidine-2,4-dione in the form of a beige-coloured solid, the characteristics of which are as follows:
후처리
- customThe solution obtained
- stirringThe reaction mixture is stirred at room temperature for 15 hours
- customthe solid formed
- filtrationis filtered off
- washwashed with three times 20 mL of water and with twice 20 mL of diethyl ether
- customdried
출처 및 근거
- ORD 기록
- ord-f78c8d64115c419ab40bdfdf6b27dc0b
- 출처 데이터셋
- uspto-grants-2011_05
- 특허 번호
- US07935819B2
연결된 노트
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