Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Dichloromethane → 2,2-Dimethylmalonic acid t-butyl ester cyclohexyl ester
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Dichloromethane | HCID 6344 | — |
| 반응물 | Cyclohexanol | HCID 7966 | — |
| 반응물 | 1-Ethyl-3-(3'-dimethylaminopropyl)carbodiimide | HCID 15908 | — |
| 반응물 | 3-(Tert-butoxy)-2,2-dimethyl-3-oxopropanoic acid | HCID 254415 | — |
| 촉매 | 4-(Dimethylamino)pyridine | HCID 14284 | — |
| 용매 | tert-Butyl methyl ether | HCID 15413 | — |
| 생성물 | 2,2-Dimethylmalonic acid t-butyl ester cyclohexyl ester | HCID 67469976 | — |
반응 단계
To a mixture of 2,2-dimethylmalonic acid mono-t-butyl ester [CAS No. 143688-40-8] (800 mg), DMAP (104 mg), and dichloromethane (8 mL), cyclohexanol (0.494 mL) and WSC (976 mg) were sequentially added at 0° C. The resulting mixture was stirred overnight at room temperature, and TBME (50 mL) was added thereto. The resulting mixture was sequentially washed with water (30 mL) and saturated aqueous sodium chloride solution (30 mL), and dried over anhydrous magnesium sulfate. The resulting mixture was filtered, and the filtrate obtained was concentrated under reduced pressure. The residue obtained was purified by silica gel column chromatography (mixed solvent of heptane-ethyl acetate) to obtain the captioned compound (817 mg).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US08436009B2 |
| 출처 데이터셋 | uspto-grants-2013_05 |
| ORD ID | ord-fa9d8e23bd104a26acf716c18aadbbc6 |
| 출처 메모 | uspto-grants-2013_05 |