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Ammonia → Perfluoroheptanamide

HRID 1810721
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HRID 1810721 반응식
[F:1][C:2]([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](OC)=[O:4].[NH3:24].[NH4+]>O1CCCC1>[F:1][C:2]([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]([NH2:24])=[O:4]
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참가 물질

5

반응물 3

HCID 222Ammonia3회HCID 223AmmoniumHCID 526471Methyl perfluoroheptanoate

생성물 1

HCID 2769670Perfluoroheptanamide수율 99%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

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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 658 g (1.74 mol) of methyl perfluoroheptanoate 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 the ammonia supply, the mixture is left to stand for 12 hr. Solvent is removed under reduced pressure, yielding 626 g p perfluoroheptanoic acid amide (99%), mp 127-128° 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-5e9656729ad34425b10541552caa1886
출처 데이터셋
uspto-grants-2013_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08362167B2

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