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

HRID 1674468ノート

反応式

HRID 1674468 の反応式
[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]

参加物

6

反応物 4

HCID 6344DichloromethaneHCID 6916Diethylcarbamoyl chlorideHCID 8471TriethylamineHCID 22481373HCID 22481373、化合物

生成物 1

HCID 866361064-(N,N-diethylaminocarboxy)phenyldiphenylsulfonium perfluorobutanesulfonate収率 152%

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-15e5337ccb1844e2992a03ad4f8b7810
出典データセット
uspto-grants-2011_08
特許番号
US08003296B2

反応ノート

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