Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Ammonia → 3-fluoro-5-o-fluorophenyl-7-nitro-2,3-dihydro-1H-1,4-benzodiazepin-2-one
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Ammonia | HCID 222 | — |
| 반응물 | Hexamethylenetetramine | HCID 4101 | — |
| 반응물 | 2-Amino-2'-fluoro-5-nitrobenzophenone | HCID 67657 | — |
| 반응물 | 2-(alpha-Bromo-alpha-fluoroacetamido)-5-nitro-2'-fluorobenzophenone | HCID 23332640 | — |
| 반응물 | alpha-Bromo-alpha-fluoroacetyl bromide | HCID 23332663 | — |
| 용매 | Ethanol | HCID 702 | — |
| 생성물 | 3-fluoro-5-o-fluorophenyl-7-nitro-2,3-dihydro-1H-1,4-benzodiazepin-2-one | HCID 23332560 | — |
반응 단계
NH3 is passed into a refluxing solution of 1.48 g. of hexamethylenetetramine in 30 ml. of ethanol; 3.83 g. of 2-(α-bromo-α-fluoroacetamido)-5-nitro-2'-fluorobenzophenone, obtainable from 2-amino-5-nitro-2'-fluorobenzophenone and α-bromo-α-fluoroacetyl bromide, are added over 2 hours. The mixture is then heated under reflux for 3 hours more and is evaporated. The resulting 2-(α-amino-α-fluoroacetamido)-5-nitro-2'-fluorobenzophenone is treated with 15 ml. of toluene and 20 mg. of p-tolunesulfonic acid and is heated under reflux for 1 hour. Working up in the customary manner gives 3-fluoro-5-o-fluorophenyl-7-nitro-2,3-dihydro-1H-1,4-benzodiazepin-2-one.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US04232016 |
| 출처 데이터셋 | uspto-grants-1980_11 |
| ORD ID | ord-5b5b4ec6a18646e5ada4fff703b054be |
| 출처 메모 | uspto-grants-1980_11 |