Triethylamine → N-Decylperfluorooctanesulfonamide

HRID 567641

反応式

HRID 567641 の反応式
[F:1][C:2]([F:29])([S:25](F)(=[O:27])=[O:26])[C:3]([F:24])([F:23])[C:4]([F:22])([F:21])[C:5]([F:20])([F:19])[C:6]([F:18])([F:17])[C:7]([F:16])([F:15])[C:8]([F:14])([F:13])[C:9]([F:12])([F:11])[F:10].C(N(CC)CC)C.[CH2:37]([NH2:47])[CH2:38][CH2:39][CH2:40][CH2:41][CH2:42][CH2:43][CH2:44][CH2:45][CH3:46]>O>[CH2:37]([NH:47][S:25]([C:2]([F:29])([F:1])[C:3]([F:23])([F:24])[C:4]([F:22])([F:21])[C:5]([F:20])([F:19])[C:6]([F:17])([F:18])[C:7]([F:15])([F:16])[C:8]([F:13])([F:14])[C:9]([F:11])([F:12])[F:10])(=[O:27])=[O:26])[CH2:38][CH2:39][CH2:40][CH2:41][CH2:42][CH2:43][CH2:44][CH2:45][CH3:46]

参加物

5

反応物 3

HCID 8471TriethylamineHCID 8916DecylamineHCID 9388Perfluorooctanesulfonyl fluoride

生成物 1

HCID 22352717N-Decylperfluorooctanesulfonamide

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

50.21 g (100.0 mmol) of perfluorooctanesulfonyl fluoride is added in drops to a mixture of 10.62 g (105.0 mmol) of triethylamine and 15.73 g (100.0 mmol) of decylamine at 80° C. while being stirred vigorously. It is stirred for 2 days at 80° C., the reaction mixture is mixed with 300 ml of water and extracted three times with ethyl acetate. The combined organic extracts are dried on sodium sulfate, filtered and concentrated by evaporation. The residue is chromatographed on silica gel (mobile solvent: dichloromethane/methanol=4/1).

後処理

  1. stirringIt is stirred for 2 days at 80° C.
  2. extractionextracted three times with ethyl acetate
  3. customThe combined organic extracts are dried on sodium sulfate
  4. filtrationfiltered
  5. concentrationconcentrated by evaporation
  6. customThe residue is chromatographed on silica gel (mobile solvent: dichloromethane/methanol=4/1)

出典と根拠

ORDレコード
ord-7fcaca3ced1f477e9b6b32890d45deff
出典データセット
uspto-grants-2001_01
特許番号
US06180113B2

関連ノート

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