Methanol → Methyl perfluorooctanoate

HRID 1810722노트

반응식

HRID 1810722 반응식
[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]

참가 물질

5

반응물 3

HCID 887MethanolHCID 1118Sulfuric AcidHCID 9554Perfluorooctanoic acid

생성물 1

HCID 67824Methyl perfluorooctanoate수율 89%

시약·촉매·용매 1

HCID 962Water용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-ccc375c16d7d412f996c223b6dc1160a
출처 데이터셋
uspto-grants-2013_01
특허 번호
US08362167B2

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