Hydrochloric Acid → (2S,3S,5R)-2-(3,4-difluorophenyl)-3,5-dimethyl-2-morpholinol hydrochloride

HRID 962903ノート

反応式

HRID 962903 の反応式
Br.[F:2][C:3]1[CH:4]=[C:5]([C@:10]2([OH:18])[O:15][CH2:14][C@@H:13]([CH3:16])[NH:12][C@H:11]2[CH3:17])[CH:6]=[CH:7][C:8]=1[F:9].[OH-].[Na+].[ClH:21]>O.CCOCC>[ClH:21].[F:2][C:3]1[CH:4]=[C:5]([C@:10]2([OH:18])[O:15][CH2:14][C@@H:13]([CH3:16])[NH:12][C@H:11]2[CH3:17])[CH:6]=[CH:7][C:8]=1[F:9]

参加物

6

反応物 3

HCID 313Hydrochloric AcidHCID 14798Sodium HydroxideHCID 67706270(2S, 3S, 5R)-2-(3,4difluorophenyl)-3,5-dimethyl-2-morpholinol hydrobromide

生成物 1

HCID 67706269(2S,3S,5R)-2-(3,4-difluorophenyl)-3,5-dimethyl-2-morpholinol hydrochloride

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 3283Diethyl Ether溶媒

実験手順

A solution of (2S, 3S, 5R)-2-(3,4-difluorophenyl)-3,5-dimethyl-2-morpholinol hydrobromide (4.85 g, 0.015 mole) in water was basified with 40% aqueous sodium hydroxide and extracted with diethyl ether. The diethyl ether layers were combined, washed with brine, dried (potassium carbonate) and concentrated under reduced pressure to yield the free base. The free base was dissolved in ether and treated with ethereal hydrogen chloride. The hydrochloride salt was recrystallized from ethanol-diethyl ether mixtures to give 3.26 g of (2S, 3S, 5R)-2-(3,4-difluorophenyl)-3,5-dimethyl-2-morpholinol hydrochloride as a white solid. m.p. 223°-225° C. dec.

後処理

  1. extractionextracted with diethyl ether
  2. washwashed with brine
  3. dry with materialdried (potassium carbonate)
  4. concentrationconcentrated under reduced pressure
  5. customto yield the free base
  6. customThe hydrochloride salt was recrystallized from ethanol-diethyl ether mixtures

出典と根拠

ORDレコード
ord-c3574abc88d348779daa99b1be24b04d
出典データセット
uspto-grants-1998_06
特許番号
US05760224

反応ノート

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