Water → HCID 19969101, 화합물

HRID 1492901

반응식

HRID 1492901 반응식
[F:1][C:2]1[C:10]([F:11])=[C:9](F)[C:8]([F:13])=[C:7]([F:14])[C:3]=1[C:4]([OH:6])=[O:5].[F:15][C:16]([F:28])([C:19]([F:27])([F:26])[C:20]([F:25])([F:24])[CH:21]([F:23])[F:22])[CH2:17][OH:18].[H-].[Na+].O>CN(C)C=O.C(OCC)(=O)C>[F:15][C:16]([F:28])([C:19]([F:26])([F:27])[C:20]([F:24])([F:25])[CH:21]([F:22])[F:23])[CH2:17][O:18][C:9]1[C:8]([F:13])=[C:7]([F:14])[C:3]([C:4]([OH:6])=[O:5])=[C:2]([F:1])[C:10]=1[F:11]

참가 물질

7

반응물 4

HCID 962WaterHCID 96412,2,3,3,4,4,5,5-Octafluoro-1-pentanolHCID 11770Pentafluorobenzoic acidHCID 24758Sodium hydride

생성물 1

HCID 19969101HCID 19969101, 화합물수율 46.2%

시약·촉매·용매 2

HCID 6228Dimethylformamide용매HCID 8857Ethyl Acetate용매

실험 절차

To a mixture of 2,3,4,5,6-pentafluorobenzoic acid (1 g) and 2,2,3,3,4,4,5,5-octafluoropentanol (1.18 g) in N,N-dimethylformamide (5 ml) was added 62% sodium hydride (0.39 g) at room temperature. The mixture was stirred at the same temperature for 1 hour, and thereto was added a mixture of water and ethyl acetate. The separated organic layer was washed with water and brine, dried over magnesium sulfate, and evaporated in vacuo. The residue was purified by chromatography on silica gel to give 4-(2,2,3,3,4,4,5,5-octafluoropentyloxy)-2,3,5,6-tetrafluorobenzoic acid (923.0 mg).

후처리

  1. additionwas added
  2. washThe separated organic layer was washed with water and brine
  3. dry with materialdried over magnesium sulfate
  4. customevaporated in vacuo
  5. customThe residue was purified by chromatography on silica gel

출처 및 근거

ORD 기록
ord-8fc2b6b69fd84eb28195c2ce3e767fe3
출처 데이터셋
uspto-grants-1994_12
특허 번호
US05376634

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