Dimethylformamide → Ethyl 3-methoxy-4-cyclohexylphenylglyoxylate

HRID 444567노트

반응식

HRID 444567 반응식
[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

참가 물질

6

반응물 4

HCID 6228Dimethylformamide2회HCID 6328Methyl iodideHCID 24758Sodium hydrideHCID 20515140HCID 20515140, 화합물

생성물 1

HCID 20515180Ethyl 3-methoxy-4-cyclohexylphenylglyoxylate

시약·촉매·용매 1

HCID 962Water용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-2505cbb7c34e413ead25b2e94889682e
출처 데이터셋
uspto-grants-1981_04
특허 번호
US04264627

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