참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Dimethylformamide | HCID 6228 | — |
| 반응물 | 1-Bromo-2-methylpropane | HCID 6555 | — |
| 반응물 | Sodium hydride | HCID 24758 | — |
| 반응물 | Triethyl ethane-1,1,2-tricarboxylate | HCID 81961 | — |
| 용매 | Water | HCID 962 | — |
| 생성물 | HCID 85546418 | HCID 85546418 | — |
반응 단계
Sodium hydride (21 gram, 0.482 mole) was added to 200 ml dimethylformamide at 20° C. under nitrogen atmosphere. Then 80 grams (0.325 mole) of triethyl ethane-1,1,2-tricarboxylate (compound [3] made in example I) was added to the solution at a temperature of below 30° C. The reaction mixture was maintained at room temperature for 4 hours and 52 ml (0.482 mole) of isobutyl bromide (R2-X) was added drop wise after which the reaction mixture was stirred for another 20 hours at room temperature. When the reaction was complete 1 liter of cold water was added and the organic materials were extracted with dichloromethane (500 ml). The organic extracts were dried over sodium sulfate filtered and evaporated to give an oily substance, which was vacuum distilled to give 88 gram (89% of the theoretical maximum yield) triethyl 4-methylpentane-1,2,2-tricarboxylate, compound [4].
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US08889898B2 |
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| 출처 데이터셋 | uspto-grants-2014_11 |
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| ORD ID | ord-e0c06348e0fe416695c8adaa9fd04713 |
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| 출처 메모 | uspto-grants-2014_11 |
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