Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Sodium Hydroxide → t-butyl (1S)-2-(3-methylphenoxy)-1-{[(3-nitrobenzyl)oxy]methyl}ethylcarbamate
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Sodium Hydroxide | HCID 14798 | — |
| 반응물 | Benzene, 1-(bromomethyl)-3-nitro- | HCID 77568 | — |
| 반응물 | Bis(tetrabutylammonium) sulphate | HCID 11433187 | — |
| 반응물 | t-butyl (1S)-2-hydroxy-1-[(3-methylphenoxy)methyl]ethylcarbamate | HCID 68697680 | — |
| 용매 | Benzene | HCID 241 | — |
| 용매 | Ethyl Acetate | HCID 8857 | — |
| 생성물 | t-butyl (1S)-2-(3-methylphenoxy)-1-{[(3-nitrobenzyl)oxy]methyl}ethylcarbamate | HCID 86609359 | 76.6% |
반응 단계
To t-butyl (1S)-2-hydroxy-1-[(3-methylphenoxy)methyl]ethylcarbamate (300 mg) obtained in Step 1 of Example 118 were added 3-nitrobenzyl bromide (254 mg), tetrabutylammonium sulfate (91 mg), benzene (2.3 ml) and 50% aqueous sodium hydroxide solution (2.3 ml), and the mixture was stirred at room temperature for 1.5 hrs. The mixture was diluted with ethyl acetate and, after washing with water, the organic layer was dried over anhydrous sodium sulfate. The solvent was evaporated and the obtained crude product was purified by silica gel chromatography (ethyl acetate-hexane) to give the title compound (340 mg).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US07728005B2 |
| 출처 데이터셋 | uspto-grants-2010_06 |
| ORD ID | ord-f3dc3c9b14454ea5a9913cceb9841054 |
| 출처 메모 | uspto-grants-2010_06 |