Methanol → Methyl 4-(2-oxopyrrolidin-1-yl)benzoate

HRID 1635551ノート

反応式

HRID 1635551 の反応式
[C:1]([C:4]1[CH:9]=[CH:8][C:7]([N:10]2[CH2:14][CH2:13][CH2:12][C:11]2=[O:15])=[CH:6][CH:5]=1)([OH:3])=[O:2].S(=O)(=O)(O)O.[CH3:21]O>>[CH3:21][O:2][C:1]([C:4]1[CH:9]=[CH:8][C:7]([N:10]2[CH2:14][CH2:13][CH2:12][C:11]2=[O:15])=[CH:6][CH:5]=1)=[O:3]

参加物

4

反応物 3

HCID 887MethanolHCID 1118Sulfuric AcidHCID 7731304-(2-Oxopyrrolidin-1-yl)benzoic acid

生成物 1

HCID 757827Methyl 4-(2-oxopyrrolidin-1-yl)benzoate収率 94%

実験手順

A mixture of 1-(4-carboxyphenyl)pyrrolidin-2-one (3.0 g, 14.6 mmol) from example 1 and sulfuric acid (0.2 mL) in 100 mL of methanol was stirred at reflux for 18 h. The solvent was removed under vacuum. The crude material was dissolved in 100 mL of ethyl acetate and the solution was washed with a saturated sodium bicarbonate solution (3×15 mL), dried and evaporated to give 3.0 g (94%) of 1-(4-methoxycarbonylphenyl)pyrrolidin-2-one as a white solid, mp 118-120° C. (chloroform/ether).

後処理

  1. temperatureat reflux for 18 h
  2. customThe solvent was removed under vacuum
  3. dissolutionThe crude material was dissolved in 100 mL of ethyl acetate
  4. washthe solution was washed with a saturated sodium bicarbonate solution (3×15 mL)
  5. customdried
  6. customevaporated

出典と根拠

ORDレコード
ord-667e29fec42d4dad823fe776988d5dde
出典データセット
uspto-grants-2003_01
特許番号
US06509359B1

反応ノート

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