Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Hydrochloric Acid → 6-Methoxy-isoquinoline 2-oxide hydrochloride
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Hydrochloric Acid | HCID 313 | — |
| 반응물 | Methanol | HCID 887 | — |
| 반응물 | m-Chloroperbenzoic acid | HCID 70297 | — |
| 반응물 | 6-Methoxyisoquinoline | HCID 11040978 | — |
| 용매 | Diethyl Ether | HCID 3283 | — |
| 용매 | Dichloromethane | HCID 6344 | — |
| 생성물 | 6-Methoxy-isoquinoline 2-oxide hydrochloride | HCID 22397332 | 80.3% |
반응 단계
At ambient temperature 133 g of m-chloroperbenzoic acid (purity 75%) was added in portions to a stirred solution of 6-methoxy-isoquinoline [Hendricks, J. B. and Rodriguez, C., J. Org. Chem. 1983, 48, 3344-3346; 79.8 g; 500 mmol] in 1.2 L of dichloromethane. Stirring was continued for 3 hours and subsequently methanol (1 L) was added. The bulk was reduced to 700 ml after which 800 ml of a saturated solution of hydrogen chloride in diethyl ether was added. Dilution with 1.5 L of diethyl ether resulted in precipitation of yellow crystals, which were separated by filtration, washed with chilled diethyl ether and dried in vacuo to give 6-methoxy-isoquinoline-N-oxide hydrochloride (85 g, 80%), (+)-FAB-MS 176 [M+H-HCl]+.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US07893088B2 |
| 출처 데이터셋 | uspto-grants-2011_02 |
| ORD ID | ord-25b9adb72939435998a8e21c12900c53 |
| 출처 메모 | uspto-grants-2011_02 |