참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Water | HCID 962 | — |
| 반응물 | Potassium Carbonate | HCID 11430 | — |
| 반응물 | Tert-butyl 5-bromopentanoate | HCID 545791 | — |
| 반응물 | 2-Chloro-5-pyrimidinol | HCID 14595700 | — |
| 용매 | Dimethyl Sulfoxide | HCID 679 | — |
| 용매 | Ethyl Acetate | HCID 8857 | — |
| 생성물 | 5-(2-Chloropyrimidin-5-yloxy)valeric acid tert-butyl ester | HCID 86636541 | 86.9% |
반응 단계
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]+.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 특허 번호 | US08084611B2 |
|---|
| 출처 데이터셋 | uspto-grants-2011_12 |
|---|
| ORD ID | ord-a51fbf98a66c4b14a4b1ddc008decf82 |
|---|
| 출처 메모 | uspto-grants-2011_12 |
|---|
