Hydrochloric Acid → 2-(2-Methoxyacetyl)-4-methylcyclohexan-1-one

HRID 621716ノート

反応式

HRID 621716 の反応式
[H-].[Na+].[CH3:3][CH:4]1[CH2:9][CH2:8][C:7](=[O:10])[CH2:6][CH2:5]1.[C:11]([O:14][CH2:15][CH2:16][O:17]C)(=O)C.Cl>C1C=CC=CC=1.O>[CH3:11][O:14][CH2:15][C:16]([CH:6]1[CH2:5][CH:4]([CH3:3])[CH2:9][CH2:8][C:7]1=[O:10])=[O:17]

参加物

7

反応物 4

HCID 313Hydrochloric AcidHCID 8054Ethylene glycol monomethyl ether acetateHCID 115254-MethylcyclohexanoneHCID 24758Sodium hydride

生成物 1

HCID 200349082-(2-Methoxyacetyl)-4-methylcyclohexan-1-one収率 87.9%

試薬・触媒・溶媒 2

HCID 241Benzene溶媒HCID 962Water溶媒

実験手順

2.5 g of 60% sodium hydride was suspended in 50 ml of benzene and a mixture of 5.6 g of 4methylcyclohexanone and 5.4 g of methoxyethyl acetate was added dropwise thereto under cooling. After stirring at room temperature for two hours, 20 ml of water was added and the pH value of the reaction mixture was adjusted to 3 with concentrated hydrochloric acid. After removing the benzene phase the aqueous phase was extracted with ether. The benzene solution and the ether solution were combined, washed with water, dried and concentrated to give 7.4 g of crude 2-methoxyacetyl4-methylcyclohexanone. This crude product was subjected to the subsequent step.

後処理

  1. additionwas added dropwise
  2. temperatureunder cooling
  3. customAfter removing the benzene phase the aqueous phase
  4. extractionwas extracted with ether
  5. washwashed with water
  6. customdried
  7. concentrationconcentrated

出典と根拠

ORDレコード
ord-6d6452be3aa04ad5abfcb8b1671e640f
出典データセット
uspto-grants-1989_04
特許番号
US04824952

反応ノート

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