Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Benzaldehyde → 3-Chloro-2-ethyl-4-(2-phenyl-1,3-dioxan-5-ylamino)-pyridine
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Benzaldehyde | HCID 240 | — |
| 반응물 | Serinol | HCID 68294 | — |
| 반응물 | p-Toluenesulfonic acid monohydrate | HCID 521998 | — |
| 반응물 | 5-Chloro-6-ethyl-4-(1,3-dihydroxy-2-propylamino)-pyridine | HCID 15346451 | — |
| 반응물 | 3,4-Dichloro-2-ethylpyridine | HCID 21708425 | — |
| 용매 | Water | HCID 962 | — |
| 용매 | Toluene | HCID 1140 | — |
| 생성물 | 3-Chloro-2-ethyl-4-(2-phenyl-1,3-dioxan-5-ylamino)-pyridine | HCID 9880046 | — |
반응 단계
2.3 g (10 mmol) of 5-chloro-6-ethyl-4-(1,3-dihydroxy-2-propylamino)-pyridine (prepared analogously to Example A from 2-amino-1,3-propanediol and 3,4-dichloro-2-ethyl-pyridine) and 5.0 g of benzaldehyde were heated with 2.1 g of p-toluenesulfonic acid hydrate in 40 ml of toluene, using a water separator, until the evolution of water had ended. Working up and purification were carried out analogously to Example A. the chromatography over silica gel (ethyl acetate) gave initially 0.6 g of trans isomer (18.8% of theory), melting point: 139-140° C., and then 2.4 g of cis isomer (75.2% of theory), melting point 119-120° C.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US06281221B1 |
| 출처 데이터셋 | uspto-grants-2001_08 |
| ORD ID | ord-986edda2c1a54907ba8a915b5cd211e7 |
| 출처 메모 | uspto-grants-2001_08 |