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

HRID 621716

반응식

HRID 621716 반응식
[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]

참가 물질

7

반응물 4

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

생성물 1

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

시약·촉매·용매 2

HCID 241Benzene용매HCID 962Water용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-6d6452be3aa04ad5abfcb8b1671e640f
출처 데이터셋
uspto-grants-1989_04
특허 번호
US04824952

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