Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Phosphorus oxychloride → 2-Chloro-5-methyl-1,3-benzoxazole
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Phosphorus oxychloride | HCID 24813 | — |
| 반응물 | Phosphorus pentachloride | HCID 24819 | — |
| 반응물 | HCID 178423563 | HCID 178423563 | — |
| 용매 | Dichloromethane | HCID 6344 | — |
| 생성물 | 2-Chloro-5-methyl-1,3-benzoxazole | HCID 9989607 | 107.6% |
반응 단계
To a suspension of 5-methylbenzo[d]oxazole-2-thiol (1.0 g, 6.1 mmol.) in POCl3 (11.7 g, 76.4 mmol.) at room temperature was added PCl5 (1.9 g, 9.15 mmol.) along with CH2Cl2 (10 mL). After 4 h of stirring at room temperature, the reaction mixture was concentrated to remove excess POCl3, and the residue was treated with Na2CO3 solution until ˜pH 8 was reached. The aqueous phase was extracted with CH2Cl2. The combined organic extracts were dried over Na2SO4, filtered and concentrated to afford 2-chloro-5-methylbenzo[d]oxazole (1.1 g crude product) which was used without further purification. MS (ESI) m/e (M+H+) 168.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US08048862B2 |
| 출처 데이터셋 | uspto-grants-2011_11 |
| ORD ID | ord-54d336af942a49dda9acf8f1a9c42fe2 |
| 출처 메모 | uspto-grants-2011_11 |