Diethyl Ether → Ethyl N-(thiophene-2-carbonyl)glycinate

HRID 2072676

反応式

HRID 2072676 の反応式
Cl.[CH2:2]([O:4][C:5](=[O:8])[CH2:6][NH2:7])[CH3:3].C(=O)([O-])[O-].[K+].[K+].CCOCC.[C:20]1([C:25](Cl)=[O:26])[S:24][CH:23]=[CH:22][CH:21]=1>O.C1C=CC=CC=1>[CH2:2]([O:4][C:5](=[O:8])[CH2:6][NH:7][C:25](=[O:26])[C:20]1[S:24][CH:23]=[CH:22][CH:21]=1)[CH3:3]

参加物

7

反応物 4

HCID 3283Diethyl EtherHCID 11430Potassium CarbonateHCID 789282-Thiophenecarbonyl chlorideHCID 2723640Glycine ethyl ester, hydrochloride

生成物 1

HCID 1720748Ethyl N-(thiophene-2-carbonyl)glycinate収率 68.4%

試薬・触媒・溶媒 2

HCID 241Benzene溶媒2 回HCID 962Water溶媒

実験手順

To a solution of glycine ethyl ester hydrochloride (22 g) and potassium carbonate (86 g) in water (600 ml) was added a mixture of benzene (600 ml) and ether (400 ml) and stirred at room temperature. 2-Thenoyl chloride (25 g) in benzene (100 ml) was added during a period of about 30 minutes under stirring and then the mixture was stirred for 2 hours at room temperature. The organic layer was separated and after dried over anhydrous sodium sulfate, concentrated under reduced pressure to give colorless crystals, which were recrystallized from ethanol to obtain the objective compound (23 g), mp 82°-83° C.

後処理

  1. stirringunder stirring
  2. stirringthe mixture was stirred for 2 hours at room temperature
  3. customThe organic layer was separated
  4. dry with materialafter dried over anhydrous sodium sulfate
  5. concentrationconcentrated under reduced pressure
  6. customto give colorless crystals, which
  7. customwere recrystallized from ethanol

出典と根拠

ORDレコード
ord-d8668908c7e54640b4194c55a0f5fa75
出典データセット
uspto-grants-1990_04
特許番号
US04914104

関連ノート

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