Carbon Dioxide → tris(pentafluoroethyl)phosphine Oxide

HRID 529190

反応式

HRID 529190 の反応式
[F:1][C:2]([P:8]([C:18]([F:24])([F:23])[C:19]([F:22])([F:21])[F:20])([C:11]([F:17])([F:16])[C:12]([F:15])([F:14])[F:13])(F)F)([F:7])[C:3]([F:6])([F:5])[F:4].C(=O)=[O:26].[PH5].[P:29]([C:44]([C:47]([F:50])([F:49])[F:48])([F:46])[F:45])([C:37]([C:40]([F:43])([F:42])[F:41])([F:39])[F:38])[C:30]([C:33]([F:36])([F:35])[F:34])([F:32])[F:31].P(O)(C(C(F)(F)F)(F)F)(C(C(F)(F)F)(F)F)=O>>[F:1][C:2]([P:8](=[O:26])([C:18]([F:24])([F:23])[C:19]([F:22])([F:21])[F:20])[C:11]([F:17])([F:16])[C:12]([F:15])([F:14])[F:13])([F:7])[C:3]([F:6])([F:5])[F:4].[P:29]([C:30]([C:33]([F:34])([F:35])[F:36])([F:31])[F:32])([C:44]([C:47]([F:50])([F:49])[F:48])([F:46])[F:45])[C:37]([C:40]([F:43])([F:42])[F:41])([F:39])[F:38]

参加物

7

反応物 5

HCID 280Carbon Dioxide3 回HCID 10287940Difluorotris(pentafluoroethyl)phosphoraneHCID 11653013Bis(pentafluoroethyl)phosphinic acidHCID 15809510Tris(pentafluoroethyl)phosphaneHCID 178527699HCID 178527699、化合物

生成物 2

HCID 11165593tris(pentafluoroethyl)phosphine OxideHCID 15809510Tris(pentafluoroethyl)phosphane

反応条件

温度
120 °C

実験手順

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.

後処理

  1. temperatureA cooled (−30° C. to −35° C.) intensive reflux condenser
  2. waitAfter 6 h
  3. temperaturethe condenser temperature is warmed to −5° C

出典と根拠

ORDレコード
ord-804b85f7ab5b4e9eaf3277b4f2db8ce3
出典データセット
uspto-grants-2016_05
特許番号
US09346838B2

関連ノート

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