참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Diethyl isopropylmalonate | HCID 12966 | — |
| 반응물 | Hexamethylphosphorous triamide | HCID 15355 | — |
| 반응물 | Sodium hydride | HCID 24758 | — |
| 반응물 | 1-Iodopropane | HCID 33643 | — |
| 용매 | Toluene | HCID 1140 | — |
| 용매 | HMPT toluene | HCID 131710867 | — |
| 생성물 | Diethyl 2-isopropyl-2-propylmalonate | HCID 599161 | 87% |
반응 단계
A solution of diethylisopropylmalonate (10.1g) in 15 ml of a 25% solution of HMPT (hexamethylphosphorus triamide) in toluene was added dropwise over 15 minutes to a suspension of sodium hydride (70 mM) in 25% HMPT/toluene (15 ml) at 50°-70° C. N-propyl iodide (17.0g) was then added over 30 minutes at 70°-100° C. and the mixture stirred at 120°-130° C. for 11/2 hours. After cooling, methylated spirits (10 ml) was added and the mixture poured onto a mixture of ice/hydrochloric acid. The product was extracted with ether, the ethereal extracts washed with sodium bicarbonate (X2), then water and dried over anhydrous magnesium sulphate. Removal of the solvent gave diethyl 2-isopropyl-2-propylmalonate as a yellow liquid b.p. 92°-94°/1 mm Hg. 87% yield.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 특허 번호 | US04042710 |
|---|
| 출처 데이터셋 | uspto-grants-1977_08 |
|---|
| ORD ID | ord-38001f5f459b49bb9047209669264c1f |
|---|
| 출처 메모 | uspto-grants-1977_08 |
|---|
