Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Acetic Anhydride → N-(2,3-dihydro-1,4-benzodioxin-5-yl)acetamide
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Acetic Anhydride | HCID 7918 | — |
| 반응물 | 2,3-Dihydro-1,4-benzodioxin-5-amine | HCID 11788387 | — |
| 용매 | Ethanol | HCID 702 | — |
| 생성물 | N-(2,3-dihydro-1,4-benzodioxin-5-yl)acetamide | HCID 658593 | 95% |
반응 단계
To a solution of 2,3-dihydrobenzo[b][1,4]dioxin-5-amine (Intermediate B3, 4.5 g, 30 mmol) in ethanol (50 mL) at room temperature was slowly added acetic anhydride (3.0 g, 30 mmol). After the addition was over, the mixture was stirred at room temperature for 5 minutes. The resulting suspension was concentrated to give the crude product, which was purified by silica gel column chromatography (petroleum ether/ethyl acetate 4/1) to afford the product N-(2,3-dihydrobenzo[b][1,4]dioxin-5-yl)acetamide (5.5 g, yield 95%). 1H NMR (400 MHz, CDCl3) δ ppm 9.12 (s, 1H), 7.44-7.46 (d, 1H, J=8.0 Hz), 6.71-6.75 (t, 1H, J=8.0 Hz), 6.59-6.61 (d, 1H, J=7.6 Hz), 4.23-4.30 (m, 4H), 2.06 (s, 3H).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US09428508B2 |
| 출처 데이터셋 | uspto-grants-2016_08 |
| ORD ID | ord-aad21df284a645318e6f503c791ea2df |
| 출처 메모 | uspto-grants-2016_08 |