Tributylamine → CH2=C(CF3)CF2Och2CF2CF3

HRID 492273ノート

反応式

HRID 492273 の反応式
C(N(CCCC)CCCC)CCC.[CH2:14]([OH:22])[C:15]([F:21])([F:20])[C:16]([F:19])([F:18])[F:17].[CH2:23]=[C:24]([C:29](OS(F)(=O)=O)([F:31])[F:30])[C:25]([F:28])([F:27])[F:26]>COCCOCCOC>[CH2:23]=[C:24]([C:29]([O:22][CH2:14][C:15]([C:16]([F:19])([F:18])[F:17])([F:21])[F:20])([F:31])[F:30])[C:25]([F:28])([F:27])[F:26]

参加物

5

反応物 3

HCID 7622TributylamineHCID 98722,2,3,3,3-PentafluoropropanolHCID 87741755CH2=C(CF3)CF2Oso2F

生成物 1

HCID 131726623CH2=C(CF3)CF2Och2CF2CF3収率 116.2%

試薬・触媒・溶媒 1

HCID 8150Diglyme溶媒

実験手順

A 100 ml flask is charged with tributylamine (15 g) and diglyme (20 ml) in a dry box. 1,1,-Dihydroperfluoropropanol (24.0 g) is added. CH2═C(CF3)CF2OSO2F (19.5 g) is added dropwise at 0-5° C. The resulting mixture is stirred at room temperature for 3 hours. The mixture is then distilled to give a liquid, which is redistilled (spinning band column) giving 27.3 g CH2═C(CF3)CF2OCH2CF2CF3, b.pt. 54° C. at 200 mm Hg. Yield is 58%. Less pure fractions are not included in the yield calculation.

後処理

  1. distillationThe mixture is then distilled
  2. customto give a liquid, which
  3. distillationis redistilled (spinning band column)

出典と根拠

ORDレコード
ord-0ee83c07885e4bc48850f422dfccaa31
出典データセット
uspto-grants-2009_05
特許番号
US07531689B2

反応ノート

読み込み中…