Methanol → Methyl perfluorooctanoate

HRID 1810722

反応式

HRID 1810722 の反応式
[F:1][C:2]([F:25])([C:6]([F:24])([F:23])[C:7]([F:22])([F:21])[C:8]([F:20])([F:19])[C:9]([F:18])([F:17])[C:10]([F:16])([F:15])[C:11]([F:14])([F:13])[F:12])[C:3]([OH:5])=[O:4].[CH3:26]O.S(=O)(=O)(O)O>O>[F:1][C:2]([F:25])([C:6]([F:23])([F:24])[C:7]([F:21])([F:22])[C:8]([F:19])([F:20])[C:9]([F:17])([F:18])[C:10]([F:15])([F:16])[C:11]([F:14])([F:13])[F:12])[C:3]([O:5][CH3:26])=[O:4]

参加物

5

反応物 3

HCID 887MethanolHCID 1118Sulfuric AcidHCID 9554Perfluorooctanoic acid

生成物 1

HCID 67824Methyl perfluorooctanoate収率 89%

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

A 2-1, four-necked, round-bottomed flask equipped with stirrer, addition funnel, thermometer and reflux condenser, is charged with 828 g (2 mol) of dried perfluorooctanoic acid, 160 g (5 mol) of methanol. The mixture is stirred and 50 ml concentrated sulfuric acid is added dropwise. Then the mixture is heated to reflux for 4 hr. At the end of the reflux period the mixture is cooled to room temperature and poured into 2 l cold water. After separation of the phases, the lower organic phase is washed with water till pH neutral and dried over CaCl2. Distillation of the crude gives 762 g (89%) of methyl perfluorooctanoate, bp 160° C.

後処理

  1. customA 2-1, four-necked, round-bottomed flask equipped with stirrer, addition funnel
  2. temperaturethermometer and reflux condenser
  3. temperatureThen the mixture is heated
  4. temperatureto reflux for 4 hr
  5. customAfter separation of the phases
  6. washthe lower organic phase is washed with water till pH neutral and
  7. dry with materialdried over CaCl2
  8. distillationDistillation of the crude

出典と根拠

ORDレコード
ord-ccc375c16d7d412f996c223b6dc1160a
出典データセット
uspto-grants-2013_01
特許番号
US08362167B2

関連ノート

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