Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Diisopropylethylamine → 2,6-Dichloro-4-(2,3-dihydro-pyrido[4,3-b][1,4]oxazin-4-sulfonyl)-phenol
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Diisopropylethylamine | HCID 81531 | — |
| 반응물 | 3,5-Dichloro-4-hydroxybenzene-1-sulfonyl chloride | HCID 2735994 | — |
| 반응물 | 2H,3H,4H-pyrido[4,3-b][1,4]oxazine | HCID 21885950 | — |
| 용매 | Tetrahydrofuran | HCID 8028 | — |
| 생성물 | 2,6-Dichloro-4-(2,3-dihydro-pyrido[4,3-b][1,4]oxazin-4-sulfonyl)-phenol | HCID 44608873 | 3.4% |
반응 단계
To a 5 ml flask, 3,4-dihydro-2H-pyrido[4,3-b][1,4]oxazine (30 mg, 0.220 mmol) was dissolved in tetrahydrofuran (3 ml). Diisopropylethylamine (0.153 ml, 0.878 mmol) was added and then stirred at 0□ for 10 minutes, and then 3,5-dichloro-4-hydroxy-benzenesulfonyl chloride (69 mg, 0.264 mmol) was added thereto and then stirred at 0□ for 1 hour. The reaction mixture was evaporated under reduced pressure. The residue was purified by column chromatography on silica eluting with a solvent of dichloromethane:ethyl acetate=1:2. The fractions containing the product were collected and evaporated to obtain the target compound 21 as pale-yellow solid (2.7 mg, 3.4%).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US08394792B2 |
| 출처 데이터셋 | uspto-grants-2013_03 |
| ORD ID | ord-5e3bd3fff7b246cfa999c83f76cefba7 |
| 출처 메모 | uspto-grants-2013_03 |