Triphenylphosphine → Triphenyl(3,3,3-trifluoropropyl)phosphanium iodide

HRID 1454080

反応式

HRID 1454080 の反応式
[F:1][C:2]([F:7])([F:6])[CH2:3][CH2:4][I:5].[C:8]1([P:14]([C:21]2[CH:26]=[CH:25][CH:24]=[CH:23][CH:22]=2)[C:15]2[CH:20]=[CH:19][CH:18]=[CH:17][CH:16]=2)[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=1>C1(C)C=CC=CC=1>[I-:5].[F:1][C:2]([F:7])([F:6])[CH2:3][CH2:4][P+:14]([C:15]1[CH:16]=[CH:17][CH:18]=[CH:19][CH:20]=1)([C:21]1[CH:26]=[CH:25][CH:24]=[CH:23][CH:22]=1)[C:8]1[CH:9]=[CH:10][CH:11]=[CH:12][CH:13]=1

参加物

4

反応物 2

HCID 11776TriphenylphosphineHCID 1561651,1,1-Trifluoro-3-iodopropane

生成物 1

HCID 19694095Triphenyl(3,3,3-trifluoropropyl)phosphanium iodide収率 92.5%

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒

実験手順

A solution of 1,1,1-trifluoro-3-iodopropane (263.1 g, 1.17 moles) and triphenylphosphine (924.4 g, 3.52 moles) in toluene (950 mL) was stirred at reflux for 12 hours. The solid product precipitated from the reaction mixture throughout the course of the reaction. The reaction was allowed to cool to ambient temperature and then cooled to about 5° C. in an ice bath. The solid precipitate was isolated by filtration and dried in vacuo at 25° C. to give a white powder (526.5 g, 92%).

後処理

  1. temperatureat reflux for 12 hours
  2. customThe solid product precipitated from the reaction mixture throughout the course of the reaction
  3. temperaturecooled to about 5° C. in an ice bath
  4. customThe solid precipitate was isolated by filtration
  5. customdried in vacuo at 25° C.

出典と根拠

ORDレコード
ord-97ed5e42eff14898b0af20e9c961caa6
出典データセット
uspto-grants-2009_01
特許番号
US07476762B2

関連ノート

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