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Ammonia → Perfluoroheptanamide

HRID 1296825
ノート
印刷プレビュー

反応式

HRID 1296825 の反応式
N.[OH-:2].[K+].[C:4]([C:23]#[N:24])([C:7]([C:10]([C:13]([C:16]([C:19]([F:22])([F:21])[F:20])([F:18])[F:17])([F:15])[F:14])([F:12])[F:11])([F:9])[F:8])([F:6])[F:5]>>[F:5][C:4]([F:6])([C:7]([F:9])([F:8])[C:10]([F:12])([F:11])[C:13]([F:15])([F:14])[C:16]([F:17])([F:18])[C:19]([F:20])([F:21])[F:22])[C:23]([NH2:24])=[O:2]
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 3

HCID 222Ammonia3 回HCID 14797Potassium HydroxideHCID 2782568Perfluoroheptanenitrile

生成物 1

HCID 2769670Perfluoroheptanamide収率 98.5%

実験手順

A ten-fold excess, fifty (50) ml, of anhydrous ammonia gas were condensed into a four-neck flask fitted with an agitator, reflux condenser, dropping funnel, thermometer, and a drying tube (filled with solid KOH) which had been cooled in a dry ice/ethanol bath. The ammonia was condensed into the flask via the drying tube. With good agitation and cooling, 60 g of a reaction product (perfluoroheptanonitrile), made in accordance with the technique described in Example 4 for conversion of a perfluoroacid to a nitrile, having the structure C6F13CN was added slowly. After addition was completed, the temperature was allowed to slowly rise to ambient allowing the excess ammonia to evaporate. The resulting white solid product was air dried to yield 62.0 g of perfluoroheptanamide having the following formula (a yield of 98.5% with a m.p. at 75-76° C.).

後処理

  1. customcondensed into a four-neck flask
  2. customfitted with an agitator
  3. temperaturereflux condenser
  4. temperaturehad been cooled in a dry ice/ethanol bath
  5. customcondensed into the flask via the drying tube
  6. temperatureWith good agitation and cooling
  7. additionwas added slowly
  8. additionAfter addition
  9. customto evaporate
  10. customdried

出典と根拠

ORDレコード
ord-c251cda011154bd3a681d1f756cf09c0
出典データセット
uspto-grants-2007_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07247749B2

反応ノート

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