Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Dimethylformamide → 3-Methoxy-5,5-dimethyl-6-oxo-5,6,7,8-tetrahydro-naphthalen-2-sulfonyl chloride
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Dimethylformamide | HCID 6228 | — |
| 반응물 | Chlorosulfonic acid | HCID 24638 | — |
| 반응물 | Oxalyl chloride | HCID 65578 | — |
| 반응물 | 7-Methoxy-1,1-dimethyl-3,4-dihydronaphthalen-2(1H)-one | HCID 13011007 | — |
| 용매 | Dichloromethane | HCID 6344 | — |
| 생성물 | 3-Methoxy-5,5-dimethyl-6-oxo-5,6,7,8-tetrahydro-naphthalen-2-sulfonyl chloride | HCID 86663820 | — |
반응 단계
To the dichloromethane (2 ml) solution of 7-methoxy-1,1-dimethyl-3,4-dihydro-1H-naphthalen-2-one (Compound A2, 200 mg, 0.980 mmol), chlorosulfonic acid (110 μl, 1.70 eq.) was added and the mixture was stirred at room temperature for 2 hr. To the reaction solution, oxalyl chloride (297 μl, 3.0 eq.) and N,N-dimethyl formamide (45 μl, 0.6 eq.) were added in three divided portions, and the mixture was stirred at room temperature for 30 min. The reaction solution was concentrated under reduced pressure to obtain the title compound (295 mg). Since the title compound is unstable, its structure was identified in the next step.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US09440922B2 |
| 출처 데이터셋 | uspto-grants-2016_09 |
| ORD ID | ord-2fa1ffd1e766470883a444cac93df6c0 |
| 출처 메모 | uspto-grants-2016_09 |