Dichloromethane → 4-(N,N-diethylaminocarboxy)phenyldiphenylsulfonium perfluorobutanesulfonate

HRID 1674468노트

반응식

HRID 1674468 반응식
[F:1][C:2]([F:17])([S:13]([O-:16])(=[O:15])=[O:14])[C:3]([F:12])([F:11])[C:4]([F:10])([F:9])[C:5]([F:8])([F:7])[F:6].O[C:19]1[CH:24]=[CH:23][C:22]([S+:25]([C:32]2[CH:37]=[CH:36][CH:35]=[CH:34][CH:33]=2)[C:26]2[CH:31]=[CH:30][CH:29]=[CH:28][CH:27]=2)=[CH:21][CH:20]=1.ClCCl.C(N(CC)[C:44](Cl)=[O:45])C.[CH2:49]([N:51](CC)[CH2:52][CH3:53])[CH3:50]>O>[F:17][C:2]([F:1])([S:13]([O-:16])(=[O:15])=[O:14])[C:3]([F:11])([F:12])[C:4]([F:10])([F:9])[C:5]([F:8])([F:7])[F:6].[CH2:49]([N:51]([O:14][C:44]([C:19]1[CH:24]=[CH:23][C:22]([S+:25]([C:32]2[CH:37]=[CH:36][CH:35]=[CH:34][CH:33]=2)[C:26]2[CH:31]=[CH:30][CH:29]=[CH:28][CH:27]=2)=[CH:21][CH:20]=1)=[O:45])[CH2:52][CH3:53])[CH3:50]

참가 물질

6

반응물 4

HCID 6344DichloromethaneHCID 6916Diethylcarbamoyl chlorideHCID 8471TriethylamineHCID 22481373HCID 22481373, 화합물

생성물 1

HCID 866361064-(N,N-diethylaminocarboxy)phenyldiphenylsulfonium perfluorobutanesulfonate수율 152%

시약·촉매·용매 1

HCID 962Water용매

실험 절차

Into a flask, 30 g of 4-hydroxyphenyldiphenylsulfonium perfluorobutanesulfonate and 300 g of dichloromethane were added to prepare a solution. In the flask, a nitrogen gas was blown. To the solution, 17.9 g of N,N-diethylcarbamoyl chloride was added and then 10.5 g of triethylamine was added thereto. The resultant mixture was stirred at room temperature for 1 hour. To the obtained reaction mixture, 100 g of ion-exchanged water was added and an organic layer was obtained by separation. The obtained organic layer was washed with 300 mL of distillated water and then dried over anhydrous magnesium sulfate. Magnesium sulfate was removed by filtration and the obtained filtrate was concentrated. The obtained residue was dried under reduced pressure to obtain 26.7 g of 4-(N,N-diethylaminocarboxy)phenyldiphenylsulfonium perfluorobutanesulfonate.

후처리

  1. customto prepare a solution
  2. additionwas added
  3. customan organic layer was obtained by separation
  4. washThe obtained organic layer was washed with 300 mL of distillated water
  5. dry with materialdried over anhydrous magnesium sulfate
  6. customMagnesium sulfate was removed by filtration
  7. concentrationthe obtained filtrate was concentrated
  8. customThe obtained residue was dried under reduced pressure

출처 및 근거

ORD 기록
ord-15e5337ccb1844e2992a03ad4f8b7810
출처 데이터셋
uspto-grants-2011_08
특허 번호
US08003296B2

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