Hydrochloric Acid → Hydrochloric Acid

HRID 1283887

反応式

HRID 1283887 の反応式
C[O:2][C:3]([C@@H:5]([NH2:12])[C:6]1[CH:11]=[CH:10][CH:9]=[CH:8][CH:7]=1)=[O:4].[ClH:13]>>[CH:9]1[CH:8]=[CH:7][C:6]([C@H:5]([NH2:12])[C:3]([OH:4])=[O:2])=[CH:11][CH:10]=1.[ClH:13]

参加物

4

実験手順

A solution of methyl L-phenylglycinate (-)-hemitartrate mono-ethanol solvate ([α]D + 62.4°, 36.888 g., 0.102 mole) in 6N-hydrochloric acid (68 ml., 0.408 mole, 4 equiv.) was refluxed for 1 hour 10 minutes and then distilled for 15 minutes. Water (68 ml.) was added and the pH of the warm solution adjusted to 7.0 with ammonium hydroxide solution (0.880, 35 ml.). The mixture was cooled in ice, filtered, and the solid was washed with water (2 × 25 ml.) and ethanol (25 ml.) and dried over phosphorus pentoxide to give L-phenylglycine as white plates (13.406 g., 87%), [α]D21 + 152.1° (c 1.007, 1N-HCl).

後処理

  1. distillationdistilled for 15 minutes
  2. additionWater (68 ml.) was added
  3. temperatureThe mixture was cooled in ice
  4. filtrationfiltered
  5. washthe solid was washed with water (2 × 25 ml.) and ethanol (25 ml.)
  6. dry with materialdried over phosphorus pentoxide

出典と根拠

ORDレコード
ord-a0bc9825e8164839830096a5db6176ac
出典データセット
uspto-grants-1976_08
特許番号
US03976680

関連ノート

読み込み中…