Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Ammonium Hydroxide → 6-bromo-8-methoxy-4,4-dimethyl-1,4-dihydro-2H-3,1-benzoxazin-2-one
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Ammonium Hydroxide | HCID 14923 | — |
| 반응물 | Bromine | HCID 24408 | — |
| 반응물 | 2H-3,1-Benzoxazin-2-one, 1,4-dihydro-4,4-dimethyl-8-methoxy- | HCID 210617 | — |
| 반응물 | Sodium Acetate | HCID 517045 | — |
| 용매 | Acetic Acid | HCID 176 | — |
| 생성물 | 6-bromo-8-methoxy-4,4-dimethyl-1,4-dihydro-2H-3,1-benzoxazin-2-one | HCID 23509642 | 93.4% |
반응 단계
To a mixture of 8-methoxy-4,4-dimethyl-1,4-dihydro-2H-3,1-benzoxazin-2-one (2.1 g, 10.1 mmol), sodium acetate (1.5 g, 18 mmol) in acetic acid (30 mL) was added bromine (0.62 mL, 12 mmol) at ambient temperature. After 30 minutes, the solution was treated with a concentrated ammonium hydroxide solution (50 mL). The precipitate was collected on a filter and washed with water (3×20 mL) to yield 6-bromo-8-methoxy-4,4-dimethyl-1,4-dihydro-2H-3,1-benzoxazin-2-one (2.7 g, 93%) as off-white solid: MS (ESI) m/z 286, 288 [M+H]+.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US06713478B2 |
| 출처 데이터셋 | uspto-grants-2004_03 |
| ORD ID | ord-57356ea393df435c9d4c129165c98866 |
| 출처 메모 | uspto-grants-2004_03 |