Ammonia → 2,2,3,3,4,4,5,5,6,6,7,7,8,8,8-Pentadecafluorooctanamide

HRID 1810723

반응식

HRID 1810723 반응식
[F:1][C:2]([F:26])([C:7]([F:25])([F:24])[C:8]([F:23])([F:22])[C:9]([F:21])([F:20])[C:10]([F:19])([F:18])[C:11]([F:17])([F:16])[C:12]([F:15])([F:14])[F:13])[C:3](OC)=[O:4].[NH3:27].[NH4+]>O1CCCC1>[F:1][C:2]([F:26])([C:7]([F:25])([F:24])[C:8]([F:23])([F:22])[C:9]([F:21])([F:20])[C:10]([F:19])([F:18])[C:11]([F:17])([F:16])[C:12]([F:15])([F:14])[F:13])[C:3]([NH2:27])=[O:4]

참가 물질

5

반응물 3

HCID 222Ammonia2회HCID 223Ammonium2회HCID 67824Methyl perfluorooctanoate

생성물 1

HCID 679192,2,3,3,4,4,5,5,6,6,7,7,8,8,8-Pentadecafluorooctanamide수율 99%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

반응 조건

온도
45 °C

실험 절차

A 3-1, four-necked, round-bottomed flask equipped with stirrer, thermometer, reflux condenser with bubble counter and inlet gas-tube, is charged with 745 g (1.74 mol) of methyl perfluorooctanoate and 1.5 l tetrahydrofurane. A stream of ammonia is passed from a pressure tank into the stirring solution. The ammonia feed rate is such that a negligible amount of gas is observed exiting the reactor as observed in the bubble counter. Temperature of the mixture increases to 40-50° C. Ammonium supply is continued until the temperature begins to decrease and an increasing volume of gas is observed exiting the reactor in the bubble counter . . . . After ending of ammonium supply, the mixture is left to stand for 12 hr. Solvent is removed under reduced pressure, yielding 712 g p perfluorooctanoic acid amide (99%), mp 136-137° C.

후처리

  1. customA 3-1, four-necked, round-bottomed flask equipped with stirrer
  2. temperaturethermometer, reflux condenser
  3. customwith bubble counter and inlet gas-tube
  4. waitthe mixture is left
  5. customSolvent is removed under reduced pressure

출처 및 근거

ORD 기록
ord-333fa3c1e9664d5bbb9d2af6a8914401
출처 데이터셋
uspto-grants-2013_01
특허 번호
US08362167B2

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