Hydrochloric Acid → HCID 86640944, 화합물

HRID 424335

반응식

HRID 424335 반응식
[CH:1]([C:3]1[CH:11]=[CH:10][C:6]([C:7](Cl)=[O:8])=[CH:5][CH:4]=1)=[CH2:2].[F:12][C:13]([F:20])([S:16]([O-:19])(=[O:18])=[O:17])[CH2:14][OH:15].[C:21]1([S+:27]([C:34]2[CH:39]=[CH:38][CH:37]=[CH:36][CH:35]=2)[C:28]2[CH:33]=[CH:32][CH:31]=[CH:30][CH:29]=2)[CH:26]=[CH:25][CH:24]=[CH:23][CH:22]=1.C(N(CC)CC)C.Cl>C(Cl)Cl>[F:12][C:13]([F:20])([S:16]([O-:19])(=[O:18])=[O:17])[CH2:14][O:15][C:7](=[O:8])[C:6]1[CH:10]=[CH:11][C:3]([CH:1]=[CH2:2])=[CH:4][CH:5]=1.[C:34]1([S+:27]([C:21]2[CH:22]=[CH:23][CH:24]=[CH:25][CH:26]=2)[C:28]2[CH:33]=[CH:32][CH:31]=[CH:30][CH:29]=2)[CH:35]=[CH:36][CH:37]=[CH:38][CH:39]=1

참가 물질

6

반응물 4

HCID 313Hydrochloric AcidHCID 8471TriethylamineHCID 110520284-Vinylbenzoyl chlorideHCID 86632756HCID 86632756, 화합물

생성물 1

HCID 86640944HCID 86640944, 화합물수율 86%

시약·촉매·용매 1

HCID 6344Dichloromethane용매2회

실험 절차

Under ice cooling, 2.0 g (12 mmol) of the 4-vinylbenzoyl chloride in methylene chloride was added dropwise to a mixture of 4.2 g (10 mmol) of triphenylsulfonium 1,1-difluoro-2-hydroxyethanesulfonate in Synthesis Example 1-13, 1.21 g (12 mmol) of triethylamine, 0.24 g (2 mmol) of N,N-dimethylaminopyridine, and 20 g of methylene chloride. The resulting mixture was stirred for 2 hours at room temperature. Thereafter, 11 g of 5% dilute hydrochloric acid was added to the reaction mixture. The organic layer was taken out and washed with water, from which methylene chloride was distilled off in vacuum. 30 g of methyl isobutyl ketone was added to the residue, which was washed with dilute aqueous ammonia and then with water. Thereafter, methyl isobutyl ketone was distilled off in vacuum. Diisopropyl ether was added to the residue. By decantation, the target compound, triphenylsulfonium 1,1-difluoro-2-(4-vinyl-benzoyloxy)-ethane-1-sulfonate was obtained. Colorless oil, 5.1 g (yield 86%). The compound has the following structure.

후처리

  1. washwashed with water, from which methylene chloride
  2. distillationwas distilled off in vacuum
  3. addition30 g of methyl isobutyl ketone was added to the residue, which
  4. washwas washed with dilute aqueous ammonia
  5. distillationThereafter, methyl isobutyl ketone was distilled off in vacuum
  6. additionDiisopropyl ether was added to the residue

출처 및 근거

ORD 기록
ord-80296f7614b5459da4bb30f95234190a
출처 데이터셋
uspto-grants-2012_01
특허 번호
US08105748B2

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