Methyl iodide → Ethyl 1-methyl-2-oxocyclopentane-1-carboxylate

HRID 58823

反応式

HRID 58823 の反応式
[O:1]=[C:2]1[CH2:6][CH2:5][CH2:4][CH:3]1[C:7]([O:9][CH2:10][CH3:11])=[O:8].[C:12]([O-])([O-])=O.[K+].[K+].CI>CC(C)=O>[CH3:12][C:3]1([C:7]([O:9][CH2:10][CH3:11])=[O:8])[CH2:4][CH2:5][CH2:6][C:2]1=[O:1]

参加物

5

反応物 3

HCID 6328Methyl iodideHCID 11430Potassium CarbonateHCID 69136Ethyl 2-oxocyclopentanecarboxylate

生成物 1

HCID 227353Ethyl 1-methyl-2-oxocyclopentane-1-carboxylate収率 92.6%

試薬・触媒・溶媒 1

HCID 180Acetone溶媒

実験手順

To a suspension of ethyl 2-oxocyclopentanecarboxylate (20.3 g, 0.130 mol) and K2CO3 (53.8 g, 0.390 mol) in acetone (90 mL) was added MeI (36.9 g, 0.250 mol) at ambient temperature. The reaction mixture was stirred for 30 min at ambient temperature and then heated under reflux for 1 h. Acetone was removed under reduced pressure and diethyl ether (200 mL) was added to the residue. The resulting mixture was stirred for 15 min and filtered. The filtrate was concentrated under reduced pressure followed by distillation under vacuum to afford ethyl 1-methyl-2-oxocyclopentanecarboxylate (20.5 g, 92% yield).

後処理

  1. temperatureheated
  2. temperatureunder reflux for 1 h
  3. customAcetone was removed under reduced pressure and diethyl ether (200 mL)
  4. additionwas added to the residue
  5. stirringThe resulting mixture was stirred for 15 min
  6. filtrationfiltered
  7. concentrationThe filtrate was concentrated under reduced pressure
  8. distillationfollowed by distillation under vacuum

出典と根拠

ORDレコード
ord-a983ff367a9f4ab487ef0b59ea207ddd
出典データセット
uspto-grants-2016_09
特許番号
US09434761B2

関連ノート

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