참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Carbon Dioxide | HCID 280 | — |
| 반응물 | Difluorotris(pentafluoroethyl)phosphorane | HCID 10287940 | — |
| 반응물 | Bis(pentafluoroethyl)phosphinic acid | HCID 11653013 | — |
| 반응물 | Tris(pentafluoroethyl)phosphane | HCID 15809510 | — |
| 반응물 | HCID 178527699 | HCID 178527699 | — |
| 생성물 | tris(pentafluoroethyl)phosphine Oxide | HCID 11165593 | — |
| 생성물 | Tris(pentafluoroethyl)phosphane | HCID 15809510 | — |
반응 단계
12.01 g (28.0 mmol) of tris(pentafluoroethyl)difluorophosphorane, (C2F5)3PF2, are initially introduced in a 100 ml glass round-bottomed flask and warmed (120° C. oil-bath temperature). A cooled (−30° C. to −35° C.) intensive reflux condenser is connected downstream of the flask. A 250 ml glass round-bottomed flask containing dry ice is connected via a T-piece so that gaseous CO2 is forced through the phosphorane liquid. The liquid is stirred at 120° C. for 6 h. In this time, a total of about 400 g (9 mol) of CO2 are bubbled through the hot liquid. After 6 h, the condenser temperature is warmed to −5° C. The clear and colourless liquid remaining (4.53 g) consists of (C2F5)3PF2 (49%), (C2F5)3P═O (49%) and (C2F5)2P(O)OH (2%). Tris(pentafluoroethyl)phosphine oxide, (C2F5)3P═O, is isolated from the reaction mixture by distillation.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 특허 번호 | US09346838B2 |
|---|
| 출처 데이터셋 | uspto-grants-2016_05 |
|---|
| ORD ID | ord-804b85f7ab5b4e9eaf3277b4f2db8ce3 |
|---|
| 출처 메모 | uspto-grants-2016_05 |
|---|
