Ethyl Acrylate → Ethyl 3-(ethoxycarbonylmethylamino)propionate

HRID 245265

反応式

HRID 245265 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 4.7 M 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, 023 mole) was added and the mixture was stirred at room temperature until completion of the reaction was ascertained by TLC. After 19 h the solution 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. customAfter 19 h the solution was partitioned with dichloromethane (3×100 mL)
  2. dry with materialThe organic layer was dried with anhydrous sodium sulfate
  3. filtrationfiltered
  4. customevaporated
  5. distillationThe residue was distilled
  6. customto afford AA (28.8 g, 61%)

出典と根拠

ORDレコード
ord-61af3afbfb5341ba8ca144a09c3b76cf
出典データセット
uspto-grants-2014_02
特許番号
US08658782B2

関連ノート

読み込み中…