Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Methanesulfonic Acid → HCID 86608136, 화합물
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Methanesulfonic Acid | HCID 6395 | — |
| 반응물 | 6-(2-Methoxy-4-{[2-(tetrahydropyran-4-yl)ethylamino]methyl}phenoxy)nicotinamide | HCID 59730141 | — |
| 용매 | Methanol | HCID 887 | — |
| 용매 | Tetrahydrofuran | HCID 8028 | — |
| 생성물 | HCID 86608136 | HCID 86608136 | 100% |
반응 단계
Dissolve 6-(2-methoxy-4-{[2-(tetrahydropyran-4-yl)ethylamino]methyl}phenoxy)nicotinamide (Example 427) (0.612, 1.59 mmol) in THF (4 mL) and few drops of methanol to form a clear solution. Add 1.27 M methanesulfonic acid (1.25 mL, 1.59 mmol) in THF. Stir for 10 minutes, then concentrate to give the title compound (0.749 g, ˜100%): TOF MS ES+ 386.2 (M+H)+, HRMS calcd for C21H25N3O4 386.2080 (M+H)+, found 386.2083, time 0.62 min; HPLC [Waters XTerra™ MS C-18 (150×4.6 mm, S-5 microm), 0.1% TFA/acetonitrile in 0.1% TFA/water at 1.0 mL/min, 5-95% over 15 min], tR=6.6 min, 100% purity.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US07531557B2 |
| 출처 데이터셋 | uspto-grants-2009_05 |
| ORD ID | ord-e63b507446934657b057885e7acea5a2 |
| 출처 메모 | uspto-grants-2009_05 |