Ethanol → HCID 22170132、化合物

HRID 1823271ノート

反応式

HRID 1823271 の反応式
C([O:3][C:4]([C:6]1[C:7]([C:12]2[CH:17]=[CH:16][N:15]=[CH:14][C:13]=2[F:18])=[N:8][O:9][C:10]=1[CH3:11])=[O:5])C.[OH-].[Na+].C(O)C>O1CCCC1>[F:18][C:13]1[CH:14]=[N:15][CH:16]=[CH:17][C:12]=1[C:7]1[C:6]([C:4]([OH:5])=[O:3])=[C:10]([CH3:11])[O:9][N:8]=1

参加物

5

反応物 3

HCID 702EthanolHCID 14798Sodium HydroxideHCID 57425437Ethyl 3-(3-Fluoro-4-pyridyl)-5-methylisoxazole-4-carboxylate

生成物 1

HCID 22170132HCID 22170132、化合物

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

Combine 3-(3-fluoro-pyridin-4-yl)-5-methyl-isoxazole-4-carboxylic acid ethyl ester (2.00 g, 0.008 mol) with aqueous sodium hydroxide (2N, 15.0 mL, 0.03 mol), ethanol (3 mL), and tetrahydrofuran (3 mL) and stir overnight at ambient temperature. Remove the organic solvents in vacuo and adjust the aqueous mixture to approx. pH 3.5 with aqueous hydrochloric acid. Extract with ethyl acetate and dry the combined extracts over sodium sulfate and concentrate in vacuo. Drying nets the desired isoxazole acid as an off white solid (1.35 g, 76%). MS(FD): M+ 223.2 m/z.

後処理

  1. customRemove the organic solvents in vacuo
  2. extractionExtract with ethyl acetate
  3. dry with materialdry the combined extracts over sodium sulfate
  4. concentrationconcentrate in vacuo
  5. customDrying

出典と根拠

ORDレコード
ord-fb9ae354fa6249f1929846597fd3dd44
出典データセット
uspto-grants-2006_05
特許番号
US07037921B2

反応ノート

読み込み中…