Benzylamine → N-Hexyl-1,1,2,2,3,3,4,4,5,5,6,6,7,7,8,8,8-heptadecafluorooctane-1-sulfonamide

HRID 376220

反応式

HRID 376220 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]([NH2:44])[C:38]1C=[CH:42][CH:41]=[CH:40][CH:39]=1>O>[CH2:37]([NH:44][S:25]([C:2]([F:1])([F:29])[C:3]([F:23])([F:24])[C:4]([F:21])([F:22])[C:5]([F:20])([F:19])[C:6]([F:17])([F:18])[C:7]([F:15])([F:16])[C:8]([F:14])([F:13])[C:9]([F:12])([F:11])[F:10])(=[O:26])=[O:27])[CH2:38][CH2:39][CH2:40][CH2:41][CH3:42]

参加物

5

反応物 3

HCID 7504BenzylamineHCID 8471TriethylamineHCID 9388Perfluorooctanesulfonyl fluoride

生成物 1

HCID 22352711N-Hexyl-1,1,2,2,3,3,4,4,5,5,6,6,7,7,8,8,8-heptadecafluorooctane-1-sulfonamide

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

50.21 g (100 mmol) of perfluorooctanesulfonyl fluoride is added in drops to a mixture of 10.62 g (105 mmol) of triethylamine and 10.12 g (100 mmol) of benzylamine 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-b0f7beb42be5483ea88e5fd84de6c17f
出典データセット
uspto-grants-2000_02
特許番号
US06019959

関連ノート

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