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

반응식

HRID 376220 반응식
[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]

참가 물질

5

반응물 3

HCID 7504BenzylamineHCID 8471TriethylamineHCID 9388Perfluorooctanesulfonyl fluoride

생성물 1

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

시약·촉매·용매 1

HCID 962Water용매

실험 절차

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).

후처리

  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)

출처 및 근거

ORD 기록
ord-b0f7beb42be5483ea88e5fd84de6c17f
출처 데이터셋
uspto-grants-2000_02
특허 번호
US06019959

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