Water → HCID 19969101、化合物

HRID 974715

反応式

HRID 974715 の反応式
[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]

参加物

7

反応物 4

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

生成物 1

HCID 19969101HCID 19969101、化合物収率 46.2%

試薬・触媒・溶媒 2

HCID 6228Dimethylformamide溶媒HCID 8857Ethyl Acetate溶媒

実験手順

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, filtered, 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).

後処理

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

出典と根拠

ORDレコード
ord-0017f2390d414d74bd6068e2c0f7ef96
出典データセット
uspto-grants-1997_03
特許番号
USH0001638

関連ノート

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