Dimethylformamide → Ethyl 3-methoxy-4-cyclohexylphenylglyoxylate

HRID 839403ノート

反応式

HRID 839403 の反応式
[H-].[Na+].[CH3:3]N(C)C=O.[OH:8][C:9]1[CH:10]=[C:11]([C:21](=[O:27])[C:22]([O:24][CH2:25][CH3:26])=[O:23])[CH:12]=[CH:13][C:14]=1[CH:15]1[CH2:20][CH2:19][CH2:18][CH2:17][CH2:16]1.CI>O>[CH3:3][O:8][C:9]1[CH:10]=[C:11]([C:21](=[O:27])[C:22]([O:24][CH2:25][CH3:26])=[O:23])[CH:12]=[CH:13][C:14]=1[CH:15]1[CH2:20][CH2:19][CH2:18][CH2:17][CH2:16]1

参加物

6

反応物 4

HCID 6228Dimethylformamide2 回HCID 6328Methyl iodideHCID 24758Sodium hydrideHCID 20515140HCID 20515140、化合物

生成物 1

HCID 20515180Ethyl 3-methoxy-4-cyclohexylphenylglyoxylate

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

To a stirred suspension of 0.01 moles of sodium hydride in 25 ml. of dry dimethylformamide which has been cooled to 0° C is added dropwise a solution of 0.01 moles of ethyl 3-hydroxy-4-cyclohexylphenylglyoxylate in 10 ml. of dimethylformamide. The reaction mixture is stirred for 15 minutes and 0.015 moles of methyliodide is then added dropwise. The mixture is allowed to stir overnight at room temperature. 200 ml. of water is added and the resulting mixture is extracted well with ether. The ether extract is washed with water, dried over sodium sulfate, evaporated to dryness and distilled to obtain ethyl 3-methoxy-4-cyclohexylphenylglyoxylate.

後処理

  1. stirringto stir overnight at room temperature
  2. extractionthe resulting mixture is extracted well with ether
  3. extractionThe ether extract
  4. washis washed with water
  5. dry with materialdried over sodium sulfate
  6. customevaporated to dryness
  7. distillationdistilled

出典と根拠

ORDレコード
ord-11e014705b764e4ca3f39c17186d5600
出典データセット
uspto-grants-1978_06
特許番号
US04094995

反応ノート

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