Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Triphenylphosphine → N,O-bis(phenoxycarbonyl)-N-(3-butyn-2-yl)hydroxylamine
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Triphenylphosphine | HCID 11776 | — |
| 반응물 | 3-Butyn-2-ol | HCID 16239 | — |
| 반응물 | Diethyl azodicarboxylate | HCID 5462977 | — |
| 반응물 | N,O-Bis-(phenoxycarbonyl)-hydroxylamine | HCID 10107329 | — |
| 용매 | Tetrahydrofuran | HCID 8028 | — |
| 생성물 | N,O-bis(phenoxycarbonyl)-N-(3-butyn-2-yl)hydroxylamine | HCID 19963272 | 88.1% |
반응 단계
To a 0° C. solution in THF (200 mL) of 3-butyn-2-ol (3.00 g, 42.9 mmol), N,O-bis(phenoxycarbonyl)hydroxylamine (11.7 g, 42.9 mmol), and triphenylphosphine (11.7 g, 42.9 mmol), was added dropwise diethylazodicarboxylate (7.40 g, 42.8 mmol). The reaction mixture was stirred for 2 hours at 0°-5° C. and then was concentrated almost to dryness. The residue was diluted with ethyl acetate, the solids were filtered off, and the flitrate was concentrated in vacuo. Chromatography on silica gel (5% ethyl acetate, pentane) provided N,O-bis(phenoxycarbonyl)-N-(3-butyn-2-yl)hydroxylamine (12.3 g, 88% ).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US05616596 |
| 출처 데이터셋 | uspto-grants-1997_04 |
| ORD ID | ord-95e13fad641345f1a3b05938a7cf3c3f |
| 출처 메모 | uspto-grants-1997_04 |