Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
1,2-Dichloroethane → 1,1-Cyclopropanedicarboxylic acid, 1,1-dimethyl ester
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | 1,2-Dichloroethane | HCID 11 | — |
| 반응물 | Dimethyl malonate | HCID 7943 | — |
| 반응물 | Potassium Carbonate | HCID 11430 | — |
| 반응물 | 4-Methylpentane-1,2-diol | HCID 91171 | — |
| 촉매 | Tetrabutylammonium Bromide | HCID 74236 | — |
| 용매 | Water | HCID 962 | — |
| 생성물 | 1,1-Cyclopropanedicarboxylic acid, 1,1-dimethyl ester | HCID 2769539 | 96.3% |
반응 단계
450.3 g of 1,2-dichloroethane (4.55 mol), 15.5 g of polyethylene glycol dimethyl ether (mean molar mass 250 g/mol) and 168.0 g of potassium carbonate (1.2 mol) were initially introduced, and the reaction mixture was heated until the 1,2-dichloroethane refluxes. 118.9 g of dimethyl malonate (0.9 mol) and 1.25 g of tetrabutylammonium bromide (3.88 mmol) were then added at the boil. The mixture was stirred using a finely dispersing stirrer (Ultra Turrax) for 6 hours. Water formed during the reaction was removed by azeotropic distillation with 1,2-dichloroethane throughout the reaction. Further work-up was carried out analogously to Comparative Example 2. The yield was 96.3%.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US06462224B2 |
| 출처 데이터셋 | uspto-grants-2002_10 |
| ORD ID | ord-1c99b871a71c46c6bb89c2767bc3272b |
| 출처 메모 | uspto-grants-2002_10 |