Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Epichlorohydrin → 4-(3-chloro-2-hydroxypropylamino)-N-methylphthalimide
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Epichlorohydrin | HCID 7835 | — |
| 반응물 | 5-amino-2-methyl-2,3-dihydro-1H-isoindole-1,3-dione | HCID 726931 | — |
| 용매 | 2,2,2-Trifluoroethanol | HCID 6409 | — |
| 생성물 | 4-(3-chloro-2-hydroxypropylamino)-N-methylphthalimide | HCID 21281736 | 77.3% |
반응 단계
Twenty-five grams (g) (0.142 mole) 4-amino-N-methylphthalimide [Flitsch, Chem. Ber. 94:2494(1961)] and 20.7 g (0.21 mole) 1-chloro-2,3-epoxypropane were added to 150 ml 2,2,2-trifluoroethanol and the reaction mixture was heated to reflux with stirring for 48 hours. Seventy to eighty ml of 2,2,2-trifluoroethanol was removed by distillation and a heavy yellow precipitate formed when the remaining solution cooled to room temperature. This precipitate was triturated with ethyl acetate, collected by filtration and dried to give 29.5 g (77% yield) of the desired phthalimide intermediate m.p. 136°-138.5° C.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US04261893 |
| 출처 데이터셋 | uspto-grants-1981_04 |
| ORD ID | ord-7b0f148de66d487c812caba10f9fd673 |
| 출처 메모 | uspto-grants-1981_04 |