関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | Tert-butyl 5-bromopentanoate | HCID 545791 | — |
| 反応物 | 2-Chloro-5-pyrimidinol | HCID 14595700 | — |
| 溶媒 | Dimethyl Sulfoxide | HCID 679 | — |
| 溶媒 | Ethyl Acetate | HCID 8857 | — |
| 生成物 | 5-(2-Chloropyrimidin-5-yloxy)valeric acid tert-butyl ester | HCID 86636541 | 86.9% |
反応手順
Potassium carbonate (2.54 g) was added to a solution of 5-bromovaleric acid tert-butyl ester (4.3 g) obtained in Reference Example 1 (1) above and 2-chloropyrimidin-5-ol (2 g) in dimethylsulfoxide (8.6 ml) and the mixture was stirred at 40° C. overnight. The reaction mixture was cooled to room temperature, water and ethyl acetate were added and the organic layer was separated, washed with a saturated brine, dried over magnesium sulfate and concentrated in vacuo. The resulting residue was purified by column chromatography (silica gel; hexane:ethyl acetate=49:1→9:1) to give 5-(2-chloropyrimidin-5-yloxy)valeric acid tert-butyl ester (3.82 g). MS (m/z): 287/289 [M+H]+.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US08084611B2 |
|---|
| 出典データセット | uspto-grants-2011_12 |
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| ORD ID | ord-a51fbf98a66c4b14a4b1ddc008decf82 |
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| 出典メモ | uspto-grants-2011_12 |
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