Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Triethylamine → 1,2-Dihydro-8-(dimethylamino)methylbenzo[b]pyrrolo[3,2,1-jk][1,2,4]triazolo[4,3-d][1,4]benzodiazepine
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Triethylamine | HCID 8471 | — |
| 반응물 | N,N-Dimethylglycine hydrazide hydrochloride | HCID 68318 | — |
| 반응물 | HCID 15132539 | HCID 15132539 | — |
| 용매 | Dimethylformamide | HCID 6228 | — |
| 생성물 | 1,2-Dihydro-8-(dimethylamino)methylbenzo[b]pyrrolo[3,2,1-jk][1,2,4]triazolo[4,3-d][1,4]benzodiazepine | HCID 67923066 | 47.2% |
반응 단계
1,2-Dihydrobenzo[b]pyrrolo[3,2,1-jk][1,4]benzodiazepin6-thione (4 g) was added to a solution of dimethylaminoacetic hydrazide hydrochloride (2 g) and triethylamine (2.4 ml) in dimethylformamide (25 ml). The mixture was refluxed overnight, cooled, and concentrated under reduced pressure. The residue was purified by high performance liquid chromatography (2.5% methano/dichloromethane). The appropriate fractions were triturated with dry ether to yield 2.4 g (47.2%) of product, mp 164°-165° C.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US05015738 |
| 출처 데이터셋 | uspto-grants-1991_05 |
| ORD ID | ord-261a1c550af5459ba45f8471822a41d2 |
| 출처 메모 | uspto-grants-1991_05 |