関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | Tributylstannane | HCID 5948 | — |
| 反応物 | Azobisisobutyronitrile | HCID 6547 | — |
| 反応物 | ethyl (RS)-2-chloro-2-[2-(1,1-dimethylethyl)pyrimidin-5-yl]-3,3-dimethylbutanoate | HCID 14718731 | — |
| 溶媒 | Toluene | HCID 1140 | — |
| 生成物 | ethyl (RS)-2-[2-(1,1-dimethylethyl)pyrimidin-5-yl]-3,3-dimethylbutanoate | HCID 14718703 | 88.3% |
反応手順
Tri-n-Butyl tin hydride (1.3 cm3) was added to a solution of ethyl (RS)-2-chloro-2-[2-(1,1-dimethylethyl)pyrimidin-5-yl]-3,3-dimethylbutanoate (1.4 g) and a catalytic amount of 2,2'-azobisisobutyronitrile in dry toluene (10 cm3). The mixture was heated to the reflux temperature for a period of 11/2 hours, after which it was cooled to the ambient temperature, poured into water, and extracted into ethyl acetate. After concentration by evaporation of the solvent under reduced pressure, the residue was subjected to column chromatography on silica gel using hexane followed by ethyl acetate as eluent to give ethyl (RS)-2-[2-(1,1-dimethyl-ethyl)pyrimidin-5-yl]-3,3-dimethylbutanoate (1.1 g) as a pale yellow liquid, the spectral data of which were identical to those obtained for the sample generated in Example 9.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US05010200 |
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| 出典データセット | uspto-grants-1991_04 |
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| ORD ID | ord-59209b8456254df4947a588a90c2d9dd |
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| 出典メモ | uspto-grants-1991_04 |
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