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

HRID 231224

反応式

HRID 231224 の反応式
[H-].[Na+].[CH3:3][CH:4]1[CH2:9][CH2:8][C:7](=[O:10])[CH2:6][CH2:5]1.[CH3:11][O:12][CH2:13][C:14](OCC)=[O:15].Cl>C1C=CC=CC=1.O>[CH3:11][O:12][CH2:13][C:14]([CH:6]1[CH2:5][CH:4]([CH3:3])[CH2:9][CH2:8][C:7]1=[O:10])=[O:15]

参加物

7

反応物 4

HCID 313Hydrochloric AcidHCID 115254-MethylcyclohexanoneHCID 24758Sodium hydrideHCID 77544Ethyl 2-methoxyacetate

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

In 50 ml of benzene was suspended 2.5 g of 60% sodium hydride. While cooling the suspension, a mixture of 5.6 g of 4-methylcyclohexanone and 5.4 g of ethyl methoxyacetate was dropwise added thereto. After stirring at room temperature for 2 hours, 20 ml of water was added thereto and the pH was rendered 3 with concentrated hyrochloric acid. The benzene phase was separated and the aqueous phase was extracted with ether. The benzene solution and the ether solution were combined with each other followed by washing with a sodium chloride aqueous solution. After drying, the mixture was concentrated to give 7.4 g of crude 2-methoxyacetyl-4-methylcyclohexanone. The crude product was used at the following step. (2) 4-Cyano-2,3,5,6,7,8-hexahydro-1-methoxymethyl-7-methyl-3-oxoisoquinoline

後処理

  1. temperatureWhile cooling the suspension
  2. additionwas dropwise added
  3. customThe benzene phase was separated
  4. extractionthe aqueous phase was extracted with ether
  5. washby washing with a sodium chloride aqueous solution
  6. customAfter drying
  7. concentrationthe mixture was concentrated

出典と根拠

ORDレコード
ord-7d7e4b78548b4ce6aea6dafc1effcb5b
出典データセット
uspto-grants-1989_07
特許番号
US04845228

関連ノート

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