Hydrochloric Acid → (RS)-5-(3-amino-phenyl)-5-methyl-morpholin-3-one hydrochloride

HRID 1929459ノート

反応式

HRID 1929459 の反応式
C(=[N:14][C:15]1[CH:16]=[C:17]([C:21]2([CH3:28])[NH:26][C:25](=[O:27])[CH2:24][O:23][CH2:22]2)[CH:18]=[CH:19][CH:20]=1)(C1C=CC=CC=1)C1C=CC=CC=1.[ClH:29]>O1CCOCC1>[ClH:29].[NH2:14][C:15]1[CH:16]=[C:17]([C:21]2([CH3:28])[NH:26][C:25](=[O:27])[CH2:24][O:23][CH2:22]2)[CH:18]=[CH:19][CH:20]=1

参加物

4

反応物 2

HCID 313Hydrochloric AcidHCID 58155203(RS)-5-[3-(benzhydrylidene-amino)-phenyl]-5-methyl-morpholin-3-one

生成物 1

HCID 66931504(RS)-5-(3-amino-phenyl)-5-methyl-morpholin-3-one hydrochloride収率 88%

試薬・触媒・溶媒 1

HCID 312751,4-Dioxane溶媒

実験手順

A solution of (RS)-5-[3-(benzhydrylidene-amino)-phenyl]-5-methyl-morpholin-3-one (5.62 g, 15 mmol) in dioxane (75 ml) was cooled to 15° C. and treated dropwise with 1 N hydrochloric acid (18 ml). The reaction mixture was stirred at room temperature overnight. For the workup, the reaction mixture was evaporated at reduced pressure, and the residue was portioned between diethylether (120 ml) and 1 N hydrochloric acid (20 ml). The aqueous phase was separated and washed with diethylether (120 ml). This procedure was repeated twice. The combined aqueous layers were evaporated at reduced pressure, and 3.27 g (88% of theory) of (RS)-5-(3-amino-phenyl)-5-methyl-morpholin-3-one hydrochloride were obtained as a yellowish solid used in the next step without further purification. Mass (calculated) C11H15ClN2O2 [242.707]; (found) [M+H]+=207.

後処理

  1. customFor the workup, the reaction mixture was evaporated at reduced pressure
  2. customThe aqueous phase was separated
  3. washwashed with diethylether (120 ml)
  4. customThe combined aqueous layers were evaporated at reduced pressure

出典と根拠

ORDレコード
ord-ac155ce95c60482a82b9faff1c9adfc1
出典データセット
uspto-grants-2012_05
特許番号
US08188079B2

反応ノート

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