alpha-(Trifluoromethyl)benzenemethanamine → (alphaR)-alpha-(Trifluoromethyl)benzenemethanamine

HRID 245143

反応式

HRID 245143 の反応式
C(O)(=O)[C@@H]([C@H](C(O)=O)O)O.[F:11][C:12]([F:22])([F:21])[CH:13]([C:15]1[CH:20]=[CH:19][CH:18]=[CH:17][CH:16]=1)[NH2:14]>C(O)(C)C>[F:11][C:12]([F:21])([F:22])[C@@H:13]([C:15]1[CH:20]=[CH:19][CH:18]=[CH:17][CH:16]=1)[NH2:14]

参加物

4

実験手順

L-Tartaric acid (36 g, 240.0 mmol) was added to a solution of 2,2,2-trifluoro-1-phenylethanamine (40 g, 228.57 mmol) in isopropanol (400 mL). The solution was heated to reflux for 30 min. The mixture was cooled and the solid was collected by filtration. The material was diluted with Na2CO3/H2O and the aqueous mixture was extracted with methylene chloride (3×100 mL). The combined organic extracts were dried over K2CO3 and concentrated under reduced pressure to afford (1R)-2,2,2-trifluoro-1-phenylethanamine (12.5 g, 31% yield) as a white solid.

後処理

  1. temperatureThe solution was heated
  2. temperatureto reflux for 30 min
  3. temperatureThe mixture was cooled
  4. filtrationthe solid was collected by filtration
  5. additionThe material was diluted with Na2CO3/H2O
  6. extractionthe aqueous mixture was extracted with methylene chloride (3×100 mL)
  7. dry with materialThe combined organic extracts were dried over K2CO3
  8. concentrationconcentrated under reduced pressure

出典と根拠

ORDレコード
ord-79dc0351029842de8514c9bcae18f474
出典データセット
uspto-grants-2014_02
特許番号
US08658636B2

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