Ethyl Acrylate → Ethyl 3-(ethoxycarbonylmethylamino)propionate

HRID 20889

反応式

HRID 20889 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>[CH2:9]([O:8][C:6]([CH2:5][NH:4][CH2:13][CH2:12][C:11]([O:15][CH2:16][CH3:17])=[O:14])=[O:7])[CH3:10]

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

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

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 AA (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
  7. customto afford AA (28.8 g, 61%)

出典と根拠

ORDレコード
ord-52b52b1c24a64847a3cd38a59d3ea0ba
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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