Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Iodine → 7-chloro-4,5-dihydro-3-(2-iodoethynyl)-5-methyl-6H-imidazo[1,5-a][1,4]benzodiazepin-6-one
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Iodine | HCID 807 | — |
| 반응물 | Sodium Hydroxide | HCID 14798 | — |
| 반응물 | 7-chloro-3-ethynyl-4,5-dihydro-5-methyl-6H-imidazo[1,5-a][1,4]benzodiazepin-6-one | HCID 19851533 | — |
| 용매 | Methanol | HCID 887 | — |
| 용매 | Water | HCID 962 | — |
| 생성물 | 7-chloro-4,5-dihydro-3-(2-iodoethynyl)-5-methyl-6H-imidazo[1,5-a][1,4]benzodiazepin-6-one | HCID 19851516 | — |
반응 단계
2.72 g (10 mmol) of 7-chloro-3-ethynyl-4,5-dihydro-5-methyl-6H-imidazo[1,5-a][1,4]benzodiazepin-6-one was suspended in 30 ml of methanol and cooled to 10°. There were then added simultaneously thereto in portions within about 10 minutes 5 ml of 28% sodium hydroxide solution and 3 g of iodine. After stirring at room temperature for 1 hour the suspension was diluted with about 30 ml of water, suction filtered and the suction filter cake was dried. By two recrystallizations from methylene chloride and ethyl acetate and from dioxane there was obtained 7-chloro-4,5-dihydro-3-(2-iodoethynyl)-5-methyl-6H-imidazo[1,5-a][1,4]benzodiazepin-6-one of melting point 215°-216°.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US04863920 |
| 출처 데이터셋 | uspto-grants-1989_09 |
| ORD ID | ord-7c5d21ccf5ea48d69ca4307184a1ac4d |
| 출처 메모 | uspto-grants-1989_09 |