Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Sulfuric acid magnesium salt (1:1) → 7-(4-chlorobenzoyl)-5-(3-chlorophenyl)-1,5-dihydro-4,1-benzothiazepin-2(3H)-one
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Sulfuric acid magnesium salt (1:1) | HCID 24083 | — |
| 반응물 | [[[2-Amino-5-(4-chlorobenzoyl)phenyl](3-chlorophenyl)methyl]thio]-acetic acid | HCID 69020567 | — |
| 용매 | Toluene | HCID 1140 | — |
| 생성물 | 7-(4-chlorobenzoyl)-5-(3-chlorophenyl)-1,5-dihydro-4,1-benzothiazepin-2(3H)-one | HCID 69019519 | 4.4% |
반응 단계
A mixture of intermediate (19) (0.079 mol) and MgSO4 (35.5 g) in toluene (500 ml) was stirred and refluxed overnight in a Dean-Stark apparatus and then cooled. The precipitate was filtered off and the filtrate was evaporated till dryness. The residue (35 g) was purified by column chromatography over silica gel (eluent: CH2Cl2/EtOAc 85/15; 20–45 μm). The pure fractions were collected and the solvent was evaporated. The residue was crystallized from acetonitrile and DIPE. The precipitate was filtered off and dried, yielding 1.5 g (4.4%) of 7-(4-chlorobenzoyl)-5-(3-chlorophenyl)-1,5-dihydro-4,1-benzothiazepin-2(3H)-one (intermediate 20), mp. 222° C.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US07153958B2 |
| 출처 데이터셋 | uspto-grants-2006_12 |
| ORD ID | ord-3a34b6d438d1495e9a8c3f4b1c0f89e4 |
| 출처 메모 | uspto-grants-2006_12 |