Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
N,N-Diethyl-2-propanamine → 5-bromo-N3-(2-chloro-3,6-difluorobenzyl)pyrazine-2,3-diamine
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | N,N-Diethyl-2-propanamine | HCID 521913 | — |
| 반응물 | 2-Amino-3,5-dibromopyrazine | HCID 620004 | — |
| 반응물 | 2-Chloro-3,6-difluorobenzylamine | HCID 2773545 | — |
| 용매 | 1-Butanol | HCID 263 | — |
| 생성물 | 5-bromo-N3-(2-chloro-3,6-difluorobenzyl)pyrazine-2,3-diamine | HCID 86659419 | 70% |
반응 단계
A solution of 2-amino-3,5-dibromopyrazine (29 mmol, 7.35 g), 2-chloro-3,6-difluorobenzylamine (29 mmol, 5.16 g), and N, N-diethylisopropylamine (32 mmol, 5.6 mL) in n-BuOH (20 mL) was refluxed for 72 hrs. After volatile components were removed on rotavap, EtOAc and water were added to the residue to facilitate the extraction. The combined organic layers were combined, dried, concentrated, and then subjected to a silica gel column chromatography by using hexanes/EtOAc (4:1) as eluents, furnishing 5-bromo-N3-(2-chloro-3,6-difluorobenzyl)pyrazine-2,3-diamine in 70% yield (7.14 g).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US08846664B2 |
| 출처 데이터셋 | uspto-grants-2014_09 |
| ORD ID | ord-d71052b2363c431a8a193624a3f04fd1 |
| 출처 메모 | uspto-grants-2014_09 |