Methanol → HCID 136127060, 화합물

HRID 432056노트

반응식

HRID 432056 반응식
[C:1](Cl)(=[O:3])C.C[OH:6].[CH3:7][O:8][N:9]=[C:10]1[C:14]2[CH:15]=[CH:16][CH:17]=[CH:18][C:13]=2[O:12][C:11]1=NO>O>[OH:12][C:13]1[CH:18]=[CH:17][CH:16]=[CH:15][C:14]=1[C:10](=[N:9][O:8][CH3:7])[C:11]([O:3][CH3:1])=[O:6]

참가 물질

5

반응물 3

HCID 887MethanolHCID 6367Acetyl chlorideHCID 178502623HCID 178502623, 화합물

생성물 1

HCID 136127060HCID 136127060, 화합물

시약·촉매·용매 1

HCID 962Water용매

실험 절차

5 g of acetyl chloride (0.064 mol) are added dropwise to 50 ml of methanol. 4.8 g (0.025 mol) of benzofuran-2,3-dione 3-(O-methyl-oxime) 2-oxime are dissolved in this mixture, and the reaction mixture is then heated under reflux for 12 hours. After cooling to room temperature, the mixture is poured into water and the product is extracted with diethyl ether. The organic phase is washed with aqueous sodium bicarbonate solution and dried over sodium sulphate, and the solvent is distilled off under reduced pressure. This gives 4.33 g of crude product which, according to HPLC, contains 27.4% methyl E-2-(2-hydroxyphenyl)-2-methoxyimino-acetate of log p=1.48 and 56% methyl Z-2-(2-hydroxyphenyl)-2-methoxyimino-acetate of log p=2.37.

후처리

  1. temperaturethe reaction mixture is then heated
  2. temperatureunder reflux for 12 hours
  3. extractionthe product is extracted with diethyl ether
  4. washThe organic phase is washed with aqueous sodium bicarbonate solution
  5. dry with materialdried over sodium sulphate
  6. distillationthe solvent is distilled off under reduced pressure

출처 및 근거

ORD 기록
ord-eede9af6374d4f108977cde411cff173
출처 데이터셋
uspto-grants-2003_12
특허 번호
US06660872B1

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