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

HRID 132764

反応式

HRID 132764 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 99.4%

試薬・触媒・溶媒 1

HCID 180Acetone溶媒

実験手順

Under vigorously agitation, 20.3 g of ethyl 2-oxocyclopentane carboxylate was added to 53.8 g of fine powdery anhydrous potassium carbonate, and after stirring for several minutes, to the mixture was added 90 ml of acetone. The reaction mixture was further stirred for 15 to 30 minutes at room temperature, then to the mixture was dropwise added 36.9 g of methyl iodide. Upon the completion of the addition, the reaction mixture was heated for reflux for 1 hour. The solvent was removed under reduced pressure, and the solid residue was washed with diethyl ether. The washing liquor was collected and washed with water. After removing the solvent, 22.0 g of pale yellow liquid was obtained. The liquid was distilled under reduced pressure, and 20.9 g of colorless liquid as a distillate cut of 131-133° C./39 mmHg was collected. Yield: 94.6%.

後処理

  1. stirringThe reaction mixture was further stirred for 15 to 30 minutes at room temperature
  2. additionUpon the completion of the addition
  3. temperaturethe reaction mixture was heated
  4. temperaturefor reflux for 1 hour
  5. customThe solvent was removed under reduced pressure
  6. washthe solid residue was washed with diethyl ether
  7. customThe washing liquor was collected
  8. washwashed with water
  9. customAfter removing the solvent

出典と根拠

ORDレコード
ord-2e8967f0cb8b4592809b590ce6d184a7
出典データセット
uspto-grants-2008_06
特許番号
US07388103B2

関連ノート

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