Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Pyridine → Carbonic acid chloromethyl ester 2,6-dibromo-4-cyanophenyl ester
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Pyridine | HCID 1049 | — |
| 반응물 | Bromoxynil | HCID 15531 | — |
| 반응물 | Chloromethyl chloroformate | HCID 62754 | — |
| 용매 | Chloroform | HCID 6212 | — |
| 생성물 | Carbonic acid chloromethyl ester 2,6-dibromo-4-cyanophenyl ester | HCID 70170999 | 94% |
반응 단계
To a suspension of 3,5-dibromo-4-hydroxybenzonitrile (10.0 g, 36.1 mmol) in 180 mL of chloroform was added pyridine (2.92 ml, 36.1 mmol). Chloromethylchloroformate (5.2 mL 60 mmol) was then added over 5 min. The mixture was allowed to stir at room temperature for 12 h. The reaction was then washed with 1% HCl aq, water, and brine. The organic layer was then dried over sodium sulfate, filtered, and evaporated to afford a white solid (12.5 g) in 94% yield. 1H-NMR (300 MHz, CDCl3) δ (ppm): 5.87 (d, 2H), 7.90 (s, 2H). 13C-NMR (300 MHz, CDCl3) δ (ppm): 73.58, 113.87, 115.68, 119.01, 136.40, 149.53, 149.71. Mp=83-85° C.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US06376548B1 |
| 출처 데이터셋 | uspto-grants-2002_04 |
| ORD ID | ord-cbf866c32fc24cc9a737db02655fd5d0 |
| 출처 메모 | uspto-grants-2002_04 |