Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Water → 2-Amino-3-(2-chloro-4,5-methylenedioxybenzyloxy)-pyridine
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Water | HCID 962 | — |
| 반응물 | 2-Amino-3-Hydroxypyridine | HCID 28114 | — |
| 반응물 | 6-Chloropiperonyl chloride | HCID 90113 | — |
| 촉매 | Trioctylmethylammonium chloride | HCID 21218 | — |
| 용매 | Dichloromethane | HCID 6344 | — |
| 용매 | Sodium Hydroxide | HCID 14798 | — |
| 생성물 | 2-Amino-3-(2-chloro-4,5-methylenedioxybenzyloxy)-pyridine | HCID 20077049 | 24.3% |
반응 단계
To a solution of 2-amino-3-hydroxypyridine (9.75 g, 0.0886 mol) in dichloromethane (55 ml) and 40% sodium hydroxide (55 ml) was added Adogen 464 (5 ml) and 6-chloropiperonyl chloride (20 g, 0,0975 mol) with vigorous stirring. The mixture was stirred at room temperature for 16 hours. Water (55 ml) was added and the mixture extracted with dichloromethane. The combined organic layers were dried and evaporated, and the residue purified by flash chromatography (silica, 1% methanol/dichloromethane) and trituration with ether to yield the title compound (6 g), m.p. 100°-104° C.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US05409943 |
| 출처 데이터셋 | uspto-grants-1995_04 |
| ORD ID | ord-c18b5067f4074f708abea2967a7af022 |
| 출처 메모 | uspto-grants-1995_04 |