Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Methanol → 2-Amino-7-hydroxyisoquinolinium 2,4,6-trimethylbenzenesulfonate
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Methanol | HCID 887 | — |
| 반응물 | 7-Isoquinolinol | HCID 459767 | — |
| 반응물 | 2-Aminoisoquinolinium Iodide | HCID 10858601 | — |
| 반응물 | O-(2,4,6-Trimethylbenzenesulfonyl)hydroxylamine | HCID 11830845 | — |
| 용매 | Diethyl Ether | HCID 3283 | — |
| 용매 | Dichloromethane | HCID 6344 | — |
| 생성물 | 2-Amino-7-hydroxyisoquinolinium 2,4,6-trimethylbenzenesulfonate | HCID 117699298 | 60.5% |
반응 단계
O-mesitylene sulfonyl hydroxylamine (MSH) (3) was used to prepare the N-amino salt as an aminating agent as described by Tamura et al., (1972) Tetrahedron Letter. 40: 4133, incorporated herein by reference in its entirety. An ice cooled solution of 7-hydroxyisoquinoline (2.0 g, 13.78 mmol) in 30 mL of dry methylene chloride, and 15 ml of dry methanol was added drop wise to O-mesitylenesulfonylhydroxylamine (2.97 g, 13.78 mmol) in 10 mL of dry methylene chloride over 5 min with stirring. The reaction stirred at 0° C. for 6 h. 70 mL of ether was added and the suspension filtered. The precipitate was recrystallized from ethyl acetate to give 2-amino-7-hydroxyisoquinolinium 2,4,6-trimethylbenzenesulfonate (6) in 60.5% yield.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US08889713B1 |
| 출처 데이터셋 | uspto-grants-2014_11 |
| ORD ID | ord-dc6594f54f0146059ab7c1b506b027da |
| 출처 메모 | uspto-grants-2014_11 |