Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Chloroform → 4-Chloro-5,6,7,8-tetrahydro[1]benzothieno[2,3-d]pyrimidin-2-amine
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Chloroform | HCID 6212 | — |
| 반응물 | Hexane | HCID 8058 | — |
| 반응물 | Phosphorus oxychloride | HCID 24813 | — |
| 반응물 | 2-Amino-5,6,7,8-tetrahydro[1]benzothieno[2,3-d]pyrimidin-4(3h)-one | HCID 290197 | — |
| 용매 | Acetic Anhydride | HCID 7918 | — |
| 생성물 | 4-Chloro-5,6,7,8-tetrahydro[1]benzothieno[2,3-d]pyrimidin-2-amine | HCID 12910200 | 44% |
반응 단계
To a 50 mL flask was added 10 (221 mg, 1 mmol) and 10 mL POCl3. The resulting mixture was refluxed for 2 h, and the solvent was removed under reduced pressure to afford a dark residue. To this was added 30 mL of CHCl3 and 300 mg of silica gel. The solvent was evaporated to afford a plug. Column chromatography of the plug with hexane: acetyl acetate=20:1 as eluent afford 105 mg (44%) of 11 as a yellow solid:
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US09056869B2 |
| 출처 데이터셋 | uspto-grants-2015_06 |
| ORD ID | ord-4357a1e6bed444b79c90c45b72e89348 |
| 출처 메모 | uspto-grants-2015_06 |