Ethyl Acrylate → Ethyl 3-(ethoxycarbonylmethylamino)propionate

HRID 20909

反応式

HRID 20909 の反応式
[OH-].[Na+].Cl.[NH2:4][CH2:5][C:6]([O:8][CH2:9][CH3:10])=[O:7].[C:11]([O:15][CH2:16][CH3:17])(=[O:14])[CH:12]=[CH2:13]>O>[CH2:16]([O:15][C:11](=[O:14])[CH2:12][CH2:13][NH:4][CH2:5][C:6]([O:8][CH2:9][CH3:10])=[O:7])[CH3:17]

参加物

5

反応物 3

HCID 8821Ethyl AcrylateHCID 14798Sodium HydroxideHCID 2723640Glycine ethyl ester, hydrochloride

生成物 1

HCID 281012Ethyl 3-(ethoxycarbonylmethylamino)propionate収率 61.6%

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

Referring to scheme 16, a 4.7M aqueous solution of sodium hydroxide (50 mL) was added into a stirred, ice-cooled solution of ethyl glycinate hydrochloride (32.19 g, 0.23 mole) in water (50 mL). Then, ethyl acrylate (23.1 g, 0.23 mole) was added and the mixture was stirred at room temperature until the completion of reaction was ascertained by TLC (19 h). After 19 h which it was partitioned with dichloromethane (3×100 mL). The organic layer was dried with anhydrous sodium sulfate, filtered and evaporated. The residue was distilled to afford 58 (28.8 g, 61%).

後処理

  1. customwas ascertained by TLC (19 h)
  2. customAfter 19 h which it was partitioned with dichloromethane (3×100 mL)
  3. dry with materialThe organic layer was dried with anhydrous sodium sulfate
  4. filtrationfiltered
  5. customevaporated
  6. distillationThe residue was distilled

出典と根拠

ORDレコード
ord-83d523f1f3ab4c6cb52549770aa930ad
出典データセット
uspto-grants-2010_06
特許番号
US07745608B2

関連ノート

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