Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Isobutylene oxide → Methyl 5-(2-hydroxy-2-methylpropoxy)-2-nitrobenzoate
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Isobutylene oxide | HCID 11208 | — |
| 반응물 | Potassium Carbonate | HCID 11430 | — |
| 반응물 | Sodium Phosphate, Monobasic, Monohydrate | HCID 516949 | — |
| 반응물 | Methyl 5-hydroxy-2-nitrobenzoate | HCID 12922678 | — |
| 용매 | Water | HCID 962 | — |
| 용매 | Acetonitrile | HCID 6342 | — |
| 생성물 | Methyl 5-(2-hydroxy-2-methylpropoxy)-2-nitrobenzoate | HCID 70099919 | 29.2% |
반응 단계
A mixture of methyl 5-hydroxy-2-nitrobenzoate (0.5 g, 2.54 mmol), 2,2-dimethyloxirane (6.86 ml, 7.61 mmol), potassium carbonate (351 mg, 2.54 mmol) and sodium dihydrogen phosphate monohydrate (350 mg, 2.54 mmol) in acetonitrile (4 ml) and water (0.6 ml) was stirred at 140° (5 bar) in a steel bomb for 6 hr. After cooling to r.t, the mixture was diluted with water, extracted with AcOEt, dried over MgSO4, filtered and evaporated. The crude product was purified by silica gel chromatography using a methylenechloride/MeOH gradient to obtain the title compound (200 mg, 29%) as light yellow viscous oil.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US08623866B2 |
| 출처 데이터셋 | uspto-grants-2014_01 |
| ORD ID | ord-10d865e4ee694388b6ecaffefeee391d |
| 출처 메모 | uspto-grants-2014_01 |