Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Sodium Hydroxide → HCID 68595558, 화합물
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Sodium Hydroxide | HCID 14798 | — |
| 반응물 | Ammonium Chloride | HCID 25517 | — |
| 반응물 | Ethanamine, 2-chloro-N-methyl-, hydrochloride (1:1) | HCID 3028223 | — |
| 반응물 | HCID 59321743 | HCID 59321743 | — |
| 촉매 | Tetrabutylammonium hydrogen sulfate | HCID 94433 | — |
| 용매 | Methanol | HCID 887 | — |
| 용매 | Acetonitrile | HCID 6342 | — |
| 생성물 | HCID 68595558 | HCID 68595558 | 23% |
반응 단계
Dissolve 3′-(4-fluoro-phenyl)-4-(1H-pyrazol-4-ylmethyl)-3,4,5,6-tetrahydro-2H-[1,2′]bipyrazinyl (0.450 g, 1.33 mmol) in acetonitrile (3 mL) and add solid sodium hydroxide (0.186 g, 4.65 mmol). After 30 min. add (2-chloro-ethyl)-methyl-amine hydrochloride (0.190 g, 1.46 mmol) and tetrabutylammonium bisulfate (18 mg, 0.0531 mmol) then reflux the mixture for 20 hr. Cool and filter the mixture then evaporate. Purify using silica gel chromatography, eluting with 6:94 2N ammonia in methanol:DCM to give a yellow oil. Dissolve the solid in methanol and add ammonium chloride then sonicate the mixture for 10 min. Evaporate the solution to give the title compound as a white solid (0.139 g, 23%). MS (ES): m/z=396 [M+H]+.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US08202873B2 |
| 출처 데이터셋 | uspto-grants-2012_06 |
| ORD ID | ord-9fc5132842d847008eb03b8a484a7813 |
| 출처 메모 | uspto-grants-2012_06 |