Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Methylamine → 3-(Methylaminomethyl)benzonitrile
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Methylamine | HCID 6329 | — |
| 반응물 | Benzonitrile, 3-(bromomethyl)- | HCID 97249 | — |
| 용매 | Tetrahydrofuran | HCID 8028 | — |
| 생성물 | 3-(Methylaminomethyl)benzonitrile | HCID 457595 | 101.4% |
반응 단계
In a 3 necked round bottom flask (250 ml), put under nitrogen atmosphere, a solution of 3-(bromomethyl)benzonitrile (5 g; 25.5 mmol; 1 eq.) in anhydrous THF (20 ml) was added dropwise into methylamine (63.76 ml; 2 M; 127.52 mmol; 5 eq.) (2M solution in THF) over 1 hour. The reaction mixture was stirred at RT for 2 hours. Some bis-benzylation was observed (7%). The reaction mixture was filtered to remove the salt. The filtrate was evaporated under reduced pressure. The residue was taken up with DCM and evaporated again to give the title compound as a yellow oil (3.78 g, quantitative yield). It was used in the next step without any further purification. LC/MS (Method B) 146.8 (M+H)+.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US09029405B2 |
| 출처 데이터셋 | uspto-grants-2015_05 |
| ORD ID | ord-b1a5c3e5b3f447bd9822a05a848b0281 |
| 출처 메모 | uspto-grants-2015_05 |