Sodium Hydroxide → HCID 17859267、化合物

HRID 1372764ノート

反応式

HRID 1372764 の反応式
[F:1][C:2]1[CH:3]=[C:4]2[C:8](=[CH:9][CH:10]=1)[N:7]([CH3:11])[CH:6]=[C:5]2[C:12]1[O:13][C:14]2[C:20]([F:21])=[C:19]([CH2:22][C:23]([O:25]C)=[O:24])[CH:18]=[CH:17][C:15]=2[N:16]=1.CCCCCC.C(OCC)(=O)C.[OH-].[Na+]>Cl>[F:1][C:2]1[CH:3]=[C:4]2[C:8](=[CH:9][CH:10]=1)[N:7]([CH3:11])[CH:6]=[C:5]2[C:12]1[O:13][C:14]2[C:20]([F:21])=[C:19]([CH2:22][C:23]([OH:25])=[O:24])[CH:18]=[CH:17][C:15]=2[N:16]=1

参加物

5

反応物 3

HCID 14798Sodium HydroxideHCID 21226206Ethyl acetate hexaneHCID 58778548HCID 58778548、化合物

生成物 1

HCID 17859267HCID 17859267、化合物収率 78%

試薬・触媒・溶媒 1

HCID 313Hydrochloric Acid溶媒

実験手順

To methyl (2-(5-fluoro-1-methyl-3-indolyl)-7-fluoro-6-benzoxazolyl)acetate (279 mg, 0.78 mmol) were added THF/methanol (1/1, 20 ml) and 0.25N NaOH (9.4 ml, 2.35 mmol). The resulting mixture was stirred at room temperature for 18 hours. The reaction mixture was poured in 1N HCl to acidify the mixture therewith, followed by extraction with chloroform/methanol (10/1). The extract was dried over anhydrous sodium sulfate, and distilled under reduced pressure to remove the solvent. The crystals thus obtained were collected by filtration under reduced pressure, washed with hexane, and dried under reduced pressure to give (2-(5-fluoro-1-methyl-3-indolyl)-7-fluoro-6-benzoxazolyl)acetic acid (208 mg, 78%) as a brown crystalline powder.

後処理

  1. extractionfollowed by extraction with chloroform/methanol (10/1)
  2. dry with materialThe extract was dried over anhydrous sodium sulfate
  3. distillationdistilled under reduced pressure
  4. customto remove the solvent
  5. customThe crystals thus obtained
  6. filtrationwere collected by filtration under reduced pressure
  7. washwashed with hexane
  8. customdried under reduced pressure

出典と根拠

ORDレコード
ord-6cf6aa2662a743b9b48dd25736319f2e
出典データセット
uspto-grants-2007_01
特許番号
US07157487B2

反応ノート

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