Acetic Acid → HCID 13302824, 화합물

HRID 1670357노트

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HRID 1670357 반응식
[CH:1]1[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.I[C:8]([F:24])([F:23])[C:9]([F:22])([F:21])[O:10][C:11]([F:20])([F:19])[C:12]([F:18])([F:17])[S:13]([F:16])(=[O:15])=[O:14].C(OOC(=O)C1C=CC=CC=1)(=O)C1C=CC=CC=1.C(O)(=O)C>O.C([O-])(=O)C.[Cu+2].C([O-])(=O)C>[C:1]1([C:8]([C:9]([O:10][C:11]([C:12]([S:13]([F:16])(=[O:14])=[O:15])([F:17])[F:18])([F:19])[F:20])([F:22])[F:21])([F:24])[F:23])[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1

참가 물질

7

반응물 4

HCID 176Acetic AcidHCID 241BenzeneHCID 7187Benzoyl PeroxideHCID 27751695-Iodoperfluoro-3-oxapentanesulfonyl fluoride

생성물 1

HCID 13302824HCID 13302824, 화합물수율 28%

시약·촉매·용매 2

HCID 8895Cupric acetate촉매HCID 962Water용매

실험 절차

7.82 g (100 mmol) of benzene, 8.52 g (20 mmol) of 5-iodooctafluoro-3-oxapentanesulfonyl fluoride, 4.84 g (20 mmol) of benzoyl peroxide, 0.36 g (2 mmol) of copper (II) acetate, and 100 mL of acetic acid were refluxed for 4 hrs at 115° C. Then the mixture was stirred at room temperature overnight. The mixture was diluted with water (˜100 mL), and the product was extracted with hexane and washed with water until neutral pH was obtained. The solvent was removed to yield dark yellow oil. The product was purified by distillation under reduced pressure (˜27 inch Hg). The first faction was composed of a mixture of the product plus iodobenzene (2.8 g, approximately 1:1 ratio). The second fraction consisted of 2.1 g of pure product (colorless oil) (28% yield).

후처리

  1. extractionthe product was extracted with hexane
  2. washwashed with water until neutral pH
  3. customwas obtained
  4. customThe solvent was removed
  5. customto yield dark yellow oil
  6. distillationThe product was purified by distillation under reduced pressure (˜27 inch Hg)
  7. additionThe first faction was composed of a mixture of the product plus iodobenzene (2.8 g, approximately 1:1 ratio)

출처 및 근거

ORD 기록
ord-066adc7b877546e78bd1dbc9b0ef0664
출처 데이터셋
uspto-grants-2011_08
특허 번호
US07993797B2

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