Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
N,N,N',N'-Tetramethylazodicarboxamide → Benzenepropanol
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | N,N,N',N'-Tetramethylazodicarboxamide | HCID 4278 | — |
| 반응물 | Tributylphosphine | HCID 13831 | — |
| 반응물 | Benzenepropanol | HCID 31234 | — |
| 반응물 | N-(tert-butoxycarbonyl)-N'-[(5-isoquinolyl)sulfonyl]-1,3-propylenediamine | HCID 21979958 | — |
| 용매 | Tetrahydrofuran | HCID 8028 | — |
| 생성물 | Benzenepropanol | HCID 31234 | — |
| 생성물 | N-(tert-butoxycarbonyl)-N'-[(5-isoquinolyl)sulfonyl]-N'-(3-phenylpropyl)-1,3-propylenediamine | HCID 21979966 | — |
반응 단계
A solution of Intermediate 1 (640 mg), 1,1′-azobis(N,N-dimethylformamide) (1200 mg, Aldrich or prepared according to Chemistry Letters, 539 (1994)) and 3-phenyl-1-propanol (710 μl, Tokyo Kasei Kogyo) in tetrahydrofuran (30 ml) was added with tri(n-butyl)phosphine (1.75 ml, Tokyo Kasei Kogyo) with stirring and ice cooling and stirred at room temperature under argon atmosphere for 13.5 hours. The precipitates in the reaction mixture were removed by filtration, and then the solvent was evaporated from the filtrate under reduced pressure. The residue was purified by flash column chromatography (hexane/ethyl acetate mixed solvent) to obtain the title compound (913 mg, mixture with a small amount of 3-phenyl-1-propanol).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US07094789B2 |
| 출처 데이터셋 | uspto-grants-2006_08 |
| ORD ID | ord-99be45a0fb164c68b4577c67d8e9e37e |
| 출처 메모 | uspto-grants-2006_08 |