참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Hydroxylamine | HCID 787 | — |
| 반응물 | N-(4-{[tert-butyl(dimethyl)silyl]oxy}butyl)-N-[3-cyano-5-cyclopropyl-2-(4-fluorophenyl)-1-benzo furan-6-yl]methanesulfonamide | HCID 89955073 | — |
| 용매 | Ethanol | HCID 702 | — |
| 생성물 | HCID 178455217 | HCID 178455217 | 84% |
반응 단계
To a 20-mL microwave tube was added a solution of Example 11B (0.1346 g, 0.242 mmol) in ethanol (3 mL) followed by hydroxylamine (50 weight % in water, 3 mL, 50.9 mmol). The tube was sealed and the thick slurry was heated in a microwave reactor (Personal Chemistry (Biotage), Emrys Creator, 300 W maximum) for 30 minutes at 140° C. The reaction mixture was concentrated in vacuo to a cloudy solution that was taken up in ethyl acetate (60 mL), washed with 10% aqueous NaCl, dried over anhydrous Na2SO4, filtered, and concentrated in vacuo to afford the title compound as a foamy white solid (0.119 g, 84%).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 특허 번호 | US09173887B2 |
|---|
| 출처 데이터셋 | uspto-grants-2015_11 |
|---|
| ORD ID | ord-1518a5620e35426ba4488c093397918c |
|---|
| 출처 메모 | uspto-grants-2015_11 |
|---|
