Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Hydrogen Bromide → 7-Hydroxy-1,1-dioxo-2,3-dihydro-1-benzothiepine-4-carboxylic acid
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Hydrogen Bromide | HCID 260 | — |
| 반응물 | Methyl 7-methoxy-1,1-dioxo-2,3-dihydro-1-benzothiepine-4-carboxylate | HCID 22990167 | — |
| 용매 | Acetic Acid | HCID 176 | — |
| 생성물 | 7-Hydroxy-1,1-dioxo-2,3-dihydro-1-benzothiepine-4-carboxylic acid | HCID 22990021 | 82.9% |
반응 단계
A mixture of methyl 7-methoxy-1,1-dioxo-2,3-dihydro-1-benzothiepine-4-carboxylate (300 mg), 48% hydrobromic acid (3 ml) and acetic acid (3 ml) was heated at reflux for 4 hours. After concentration under reduced pressure, 48% hydrobromic acid (3 ml) and acetic acid (3 ml) were further added to the reaction mixture, which was heated at reflux for 8 hours. After concentration under reduced pressure, the precipitated crystals were collected by filtration. The crystals were washed with diisopropyl ether to obtain 7-hydroxy-1,1-dioxo-2,3-dihydro-1-benzothiepine-4-carboxylic acid (224 mg) as light yellow crystals.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US06627651B1 |
| 출처 데이터셋 | uspto-grants-2003_09 |
| ORD ID | ord-813649f0bd4d455fb8dab86a688e78af |
| 출처 메모 | uspto-grants-2003_09 |