Pyridine → 3-(6-Methyl-pyridin-2-yl)-3-(2-oxo-pyrrolidin-1-ylimino)-propionic Acid Ethyl Ester

HRID 2221144ノート

反応式

HRID 2221144 の反応式
Cl.[NH2:2][N:3]1[CH2:7][CH2:6][CH2:5][C:4]1=[O:8].[CH2:9]([O:11][C:12](=[O:23])[CH2:13][C:14]([C:16]1[CH:21]=[CH:20][CH:19]=[C:18]([CH3:22])[N:17]=1)=O)[CH3:10].N1C=CC=CC=1>O>[CH2:9]([O:11][C:12](=[O:23])[CH2:13][C:14]([C:16]1[CH:21]=[CH:20][CH:19]=[C:18]([CH3:22])[N:17]=1)=[N:2][N:3]1[CH2:7][CH2:6][CH2:5][C:4]1=[O:8])[CH3:10]

参加物

5

反応物 3

HCID 1049PyridineHCID 219928451-Aminopyrrolidin-2-one hydrochlorideHCID 59710028Ethyl 3-(6-methylpyridin-2-yl)-3-oxopropanoate

生成物 1

HCID 597100333-(6-Methyl-pyridin-2-yl)-3-(2-oxo-pyrrolidin-1-ylimino)-propionic Acid Ethyl Ester

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

Add 1-aminopyrrolidin-2-one hydrochloride (Zubek, A. Z. Chem. 1969, 9(2), 58; 99.4 g, 0.73 mol) to a 3 L flask equipped with mechanical stirrer and nitrogen inlet. Add 3-[6-methyl-(pyridin-2-yl)]-3-oxo-propionic acid ethyl ester (154 g, 0.66 mol), and pyridine (280 mL). Stir the reaction mixture at room temperature for 20 h. Dilute the mixture with water (200 mL) and extract with toluene (2×250 mL). Combine the organic layers, filter, and concentrate in vacuo to yield the subtitled product (201 g) as a dark oil. MS ES+ m/e 290 (M+1).

後処理

  1. custom99.4 g, 0.73 mol) to a 3 L flask equipped with mechanical stirrer and nitrogen inlet
  2. extractionextract with toluene (2×250 mL)
  3. filtrationCombine the organic layers, filter
  4. concentrationconcentrate in vacuo

出典と根拠

ORDレコード
ord-c12874eff9284e05a25ef5a8a9f8189a
出典データセット
uspto-grants-2008_05
特許番号
US07368445B2

反応ノート

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