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Itaconic acid → HCID 86658305、化合物

HRID 2402762
ノート
印刷プレビュー

反応式

HRID 2402762 の反応式
[C:1]([OH:9])(=[O:8])[C:2]([CH2:4][C:5]([OH:7])=[O:6])=[CH2:3].CN.C(C1C[N:18](C)[C:17](=O)C1)(O)=O>O>[C:1]([OH:9])(=[O:8])[C:2]([CH2:4][C:5]([OH:7])=[O:6])=[CH2:3].[CH3:17][NH2:18]
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 811Itaconic acid2 回HCID 6329MethylamineHCID 1227661-Methyl-5-oxopyrrolidine-3-carboxylic acid

生成物 1

HCID 86658305HCID 86658305、化合物収率 67%

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

Itaconic acid (100 g, 0.78 mol) and methylamine (41% in water, 60.0 g based on the aqueous solution, 0.80 mol, 1.0 equivalent) were mixed as in example 8. The suspension was heated to boiling under reflux at standard pressure for 1 hour (in the course of which the boiling point rises to approx. 115° C.). This dissolved the solids completely. Cooling to ambient temperature formed a precipitate. NMR analysis of the homogeneous solution and of the precipitated crystals (solvent: D2O) showed that the itaconic acid:4-carboxy-1-methylpyrrolidone ratio in both phases was 0:100. The 4-carboxy-1-methylpyrrolidone product was purified by recrystallization from ethyl acetate and was obtained in the form of colorless crystals (yield: 59 g, 67%).

後処理

  1. additionwere mixed as in example 8
  2. temperatureThe suspension was heated
  3. temperatureunder reflux at standard pressure for 1 hour (in the course of which the boiling point
  4. customrises to approx. 115° C.
  5. dissolutionThis dissolved the solids completely
  6. customformed a precipitate
  7. customThe 4-carboxy-1-methylpyrrolidone product was purified by recrystallization from ethyl acetate

出典と根拠

ORDレコード
ord-6eb2071a5ea64ffb98dd51b68213eff3
出典データセット
uspto-grants-2014_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08796472B2

反応ノート

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このページの内容参加物実験手順後処理出典と根拠反応ノート