Dimethyl itaconate → Methyl 1-(4-methoxybenzyl)-5-oxopyrrolidine-3-carboxylate

HRID 715925

反応式

HRID 715925 の反応式
[CH3:1][O:2][C:3]1[CH:8]=[CH:7][C:6]([CH2:9][NH2:10])=[CH:5][CH:4]=1.[C:11]([O:20][CH3:21])(=[O:19])[C:12]([CH2:14][C:15](OC)=[O:16])=[CH2:13]>C(OCC)(=O)C>[CH3:1][O:2][C:3]1[CH:8]=[CH:7][C:6]([CH2:9][N:10]2[C:15](=[O:16])[CH2:14][CH:12]([C:11]([O:20][CH3:21])=[O:19])[CH2:13]2)=[CH:5][CH:4]=1

参加物

4

反応物 2

HCID 69240Dimethyl itaconateHCID 754524-Methoxybenzylamine

生成物 1

HCID 4093874Methyl 1-(4-methoxybenzyl)-5-oxopyrrolidine-3-carboxylate収率 96.6%

試薬・触媒・溶媒 1

HCID 8857Ethyl Acetate溶媒

反応条件

温度
120 °C

実験手順

A mixture of (4-methoxyphenyl)methanamine (6.9 g) and dimethyl itaconate (7.9 g) was stirred at 120° C. for 2 hours. After cooling, ethyl acetate was added to the reaction solution. The organic layer was washed with 1 N hydrochloric acid, a saturated aqueous solution of sodium bicarbonate, and saturated saline in this order and then dried over anhydrous sodium sulfate. The solvent was distilled off under reduced pressure to obtain the title compound (12.7 g).

後処理

  1. temperatureAfter cooling
  2. washThe organic layer was washed with 1 N hydrochloric acid
  3. dry with materiala saturated aqueous solution of sodium bicarbonate, and saturated saline in this order and then dried over anhydrous sodium sulfate
  4. distillationThe solvent was distilled off under reduced pressure

出典と根拠

ORDレコード
ord-73eb7d946786429985ec642fa29e92f9
出典データセット
uspto-grants-2015_11
特許番号
US09187489B2

関連ノート

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