Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Sodium borohydride → 5-ethoxycarbonylmethyl-7-chloro-1-[2-methyl-4-(2-methylbenzoylamino)benzoyl]-2,3,4,5-tetrahydro-1H-benzazepine
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Sodium borohydride | HCID 4311764 | — |
| 반응물 | 5-ethoxycarbonylmethylidene-7-chloro-1-[2-methyl-4-(2-methylbenzoylamino)benzoyl]-2,3,4,5-tetrahydro-1H-benzazepine | HCID 54237705 | — |
| 촉매 | Dichloronickel;hexahydrate | HCID 11791229 | — |
| 용매 | MeOH tetrahydrofuran | HCID 21899815 | — |
| 생성물 | 5-ethoxycarbonylmethyl-7-chloro-1-[2-methyl-4-(2-methylbenzoylamino)benzoyl]-2,3,4,5-tetrahydro-1H-benzazepine | HCID 18917316 | 43.2% |
반응 단계
5-Ethoxycarbonylmethylidene-7-chloro-1-[2-methyl-4-(2-methylbenzoylamino)benzoyl]-2,3,4,5-tetrahydro-1H-benzazepine (0.30 g) and nickel chloride hexahydrate (0.55 g) are dissolved in a mixture of tetrahydrofuran/methanol (1:1) (30 ml), and to the mixture is added slowly sodium borohydride (0.26 g) with stirring under ice-cooling, and then the mixture is further stirred for 10 minutes under ice-cooling. The insoluble materials are filtered with Celite, and the filtrate is concentrated. The resulting residue is purified by silica gel column chromatography (eluent; ethyl acetate:n-hexane=1:1) to give 5-ethoxycarbonylmethyl-7-chloro-1-[2-methyl-4-(2-methylbenzoylamino)benzoyl]-2,3,4,5-tetrahydro-1H-benzazepine (0.13 g) as colorless amorphous.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US05244898 |
| 출처 데이터셋 | uspto-grants-1993_09 |
| ORD ID | ord-be3698e1a0504a98b5ed49a7b8e68b9f |
| 출처 메모 | uspto-grants-1993_09 |