Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Hydrochloric Acid → Ethyl 4-(2-(1,3-dihydro-1,3-dioxo-2H-isoindol-2-yl)ethoxy)-3-oxobutanoate
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Hydrochloric Acid | HCID 313 | — |
| 반응물 | Sodium hydride | HCID 24758 | — |
| 반응물 | Ethyl 4-chloroacetoacetate | HCID 69484 | — |
| 반응물 | N-(2-Hydroxyethyl)phthalimide | HCID 77499 | — |
| 용매 | Tetrahydrofuran | HCID 8028 | — |
| 용매 | Ethyl Acetate | HCID 8857 | — |
| 생성물 | Ethyl 4-(2-(1,3-dihydro-1,3-dioxo-2H-isoindol-2-yl)ethoxy)-3-oxobutanoate | HCID 9840027 | 97.1% |
반응 단계
To a slurry of sodium hydride (57% dispersion in oil, 66.1 g; 1.57M), in tetrahydrofuran (500 ml) cooled to 0° under nitrogen was added B 2-phthalimidoethanol (150 g; 0.785M) followed by ethyl 4-chloroacetoacetate (129 g; 0.785M) in tetrahydrofuran (250 ml) over 1 hour. The mixture was stirred at room temperature overnight then poured into a mixture of 1M hydrochloric acid (800 ml) and ethyl acetate (750 ml). The organic phase was separated and the solvent was evaporated at reduced pressure. The residue separated into two layers and the upper layer of mineral oil was removed to leave the title compound (243 g) as a crude product which was used without further purification.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US04572908 |
| 출처 데이터셋 | uspto-grants-1986_02 |
| ORD ID | ord-aed0766853a64c078285fc0008c5d1ca |
| 출처 메모 | uspto-grants-1986_02 |