참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Diisopropylethylamine | HCID 81531 | — |
| 반응물 | 2-Hydrazinyl-N,N-dimethylethanamine | HCID 120552 | — |
| 반응물 | 9-Fluoro-6-(p-toluenesulfonyloxy)benzo[g]isoquinoline-5,10-dione | HCID 10572880 | — |
| 반응물 | 9-Chloro-6-(p-toluenesulfonyloxy)benzo[g]isoquinoline-5,10-dione | HCID 19974754 | — |
| 용매 | Water | HCID 962 | — |
| 용매 | Tetrahydrofuran | HCID 8028 | — |
| 생성물 | HCID 178427630 | HCID 178427630 | — |
반응 단계
Under a nitrogen atmosphere a solution of 2-(dimethylaminoethyl)hydrazine (J. Med. Chem. 7, 493, 1964) (1.86 g) in anhydrous THF (6.0 mL) is added during 30' to the stirred 9:1 mixture of 9-fluoro-6-(p-toluenesulfonyloxy)benzo[g]isoquinoline-5,10-dione and 9-chloro-6-(p-toluenesulfonyloxy)benzo[g]isoquinoline-5,10-dione of Preparative Example 10b (2.4 g) in THF (24 mL) containing N,N-diisopropylethylamine (1.10 mL). A slightly exothermic reaction ensues, and the reaction temperature increases from 20° C. to 25° C. After one hour at room temperature the reaction mixture is poured in water (240 mL) and the suspension obtained is stirred for 30'. The solid is separated by suction, washed with water and dried at 40° C. to give 2-[2-(dimethylamino)ethyl)]-5-(p-toluenesulfonyloxy)isoquino[8,7,6-cd]indazole-6(2H)-one (1.44 g).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 특허 번호 | US05519029 |
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| 출처 데이터셋 | uspto-grants-1996_05 |
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| ORD ID | ord-127deb16558d4906b4e0c73267926d33 |
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| 출처 메모 | uspto-grants-1996_05 |
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