Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Triphenylphosphine → 1,4,7,10,13,16-Hexaoxacyclooctadecane-2,8,14-trione
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Triphenylphosphine | HCID 11776 | — |
| 반응물 | Diethyl azodicarboxylate | HCID 5462977 | — |
| 반응물 | Toluene methylene chloride | HCID 21877217 | — |
| 반응물 | 17-Hydroxy-7,13-dioxo-3,6,9,12,15-pentaoxaheptadecan-1-oic acid | HCID 86674060 | — |
| 용매 | Toluene | HCID 1140 | — |
| 생성물 | 1,4,7,10,13,16-Hexaoxacyclooctadecane-2,8,14-trione | HCID 86674059 | 61.3% |
반응 단계
To a stirred solution of triphenylphosphine (4.68 g, 17.85 mmol) in a dichloromethane/toluene 1/1 mixture (1.5 l) was added at room temperature DEAD (8.2 ml, 44.63 mmol). Reaction mixture stirred at room temperature for 10 min then a toluene solution of hydroxyacid 12 (1.18 g, 3.57 mmol) was added. Mixture was stirred at room temperature and concentrated. Careful flash chromatography on silica gel (EtOAc/pentane 1/1 then 2/1 then EtOAc 100%) afforded cyclic 14 as a white solid (670 mg, 60%).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US08624044B2 |
| 출처 데이터셋 | uspto-grants-2014_01 |
| ORD ID | ord-9d654bc7f88647ac934c06beb80eb89f |
| 출처 메모 | uspto-grants-2014_01 |