Water → HCID 86596790、化合物

HRID 1351054ノート

反応式

HRID 1351054 の反応式
[F:1][C:2]([F:17])([F:16])[C:3]([F:15])([F:14])[C:4]([F:13])([F:12])[C:5]([F:11])([F:10])[S:6]([O-:9])(=[O:8])=[O:7].[OH:18][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.[F:38][C:39]([F:54])([S:50](Cl)(=[O:52])=[O:51])[C:40]([F:49])([F:48])[CH:41]1[CH2:46][CH:45]2[CH2:47][CH:42]1[CH2:43][CH2:44]2.C(N(CC)CC)C.O>ClCCl>[F:17][C:2]([F:1])([F:16])[C:3]([F:14])([F:15])[C:4]([F:12])([F:13])[C:5]([F:10])([F:11])[S:6]([O-:9])(=[O:8])=[O:7].[F:54][C:39]([F:38])([S:50]([O:18][C:19]1[CH:24]=[CH:23][C:22]([S+:25]([C:32]2[CH:33]=[CH:34][CH:35]=[CH:36][CH:37]=2)[C:26]2[CH:31]=[CH:30][CH:29]=[CH:28][CH:27]=2)=[CH:21][CH:20]=1)(=[O:52])=[O:51])[C:40]([F:48])([F:49])[CH:41]1[CH2:46][CH:45]2[CH2:47][CH:42]1[CH2:43][CH2:44]2

参加物

6

反応物 4

HCID 962WaterHCID 8471TriethylamineHCID 22481373HCID 22481373、化合物HCID 86596792HCID 86596792、化合物

生成物 1

HCID 86596790HCID 86596790、化合物収率 54.2%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

30 g of 4-hydroxyphenyl diphenylsulfonium nonafluoro-n-butanesulfonate was dissolved in 300 g of dichloromethane in a reaction flask, in which the atmosphere was replaced with nitrogen. 30.6 g of 1,1,2,2-tetrafluoro-2-(norbornan-2-yl)ethanesulfonyl chloride and 10.5 g of triethylamine were added in this order. The mixture was stirred for 20 minutes at room temperature. After the addition of 100 g of ion-exchanged water, the mixture was transferred to a separatory funnel, shaken, and allowed to stand still. The water layer was removed. After the addition of 300 ml of distilled water, the solution was shaken and allowed to stand still. The water layer was removed. The resulting dichloromethane solution was dried using anhydrous magnesium sulfate and filtered. After evaporating dichloromethane from the dichloromethane solution, the residual liquid was dried under reduced pressure to obtain 23.5 g of 4-[1,1,2,2-tetrafluoro-2-(norbornan-2-yl)ethanesulfonyloxy]phenyl diphenylsulfonium nonafluoro-n-butanesulfonate. This compound is indicated as “acid generator (A-3)”.

後処理

  1. customthe mixture was transferred to a separatory funnel
  2. stirringshaken
  3. customThe water layer was removed
  4. additionAfter the addition of 300 ml of distilled water
  5. stirringthe solution was shaken
  6. customThe water layer was removed
  7. dry with materialThe resulting dichloromethane solution was dried
  8. filtrationfiltered
  9. customAfter evaporating dichloromethane from the dichloromethane solution
  10. customthe residual liquid was dried under reduced pressure

出典と根拠

ORDレコード
ord-65bd5fdb074049c9a5a508f18d6149cc
出典データセット
uspto-grants-2007_05
特許番号
US07217492B2

反応ノート

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