Water → 4-n-Butanesulfonyloxyphenyl diphenylsulfonium nonafluoro-n-butanesulfonate

HRID 1351053노트

반응식

HRID 1351053 반응식
[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.[CH2:38]([S:42](Cl)(=[O:44])=[O:43])[CH2:39][CH2:40][CH3:41].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].[CH2:38]([S:42]([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:44])=[O:43])[CH2:39][CH2:40][CH3:41]

참가 물질

6

반응물 4

HCID 962WaterHCID 8471TriethylamineHCID 754301-Butanesulfonyl chlorideHCID 22481373HCID 22481373, 화합물

생성물 1

HCID 865967884-n-Butanesulfonyloxyphenyl diphenylsulfonium nonafluoro-n-butanesulfonate수율 73.7%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

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. 17.9 g of n-butanesulfonyl 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 26.7 g of 4-n-butanesulfonyloxyphenyl diphenylsulfonium nonafluoro-n-butanesulfonate. This compound is indicated as “acid generator (A-1)”.

후처리

  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

출처 및 근거

ORD 기록
ord-bf06902f67be405c9d048e256c4a904b
출처 데이터셋
uspto-grants-2007_05
특허 번호
US07217492B2

반응 노트

불러오는 중…