Bicarbonate Ion → HCID 136127060, 화합물

HRID 432051노트

반응식

HRID 432051 반응식
[OH:1][C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][C:3]=1[C:8](=[N:13][OH:14])[C:9]([O:11][CH3:12])=[O:10].[C:15](=O)(O)[O-].S(OC)(OC)(=O)=O.O>C(#N)C>[OH:1][C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][C:3]=1[C:8](=[N:13][O:14][CH3:15])[C:9]([O:11][CH3:12])=[O:10]

참가 물질

6

반응물 4

HCID 769Bicarbonate IonHCID 962WaterHCID 6497Dimethyl SulfateHCID 136388365HCID 136388365, 화합물

생성물 1

HCID 136127060HCID 136127060, 화합물

시약·촉매·용매 1

HCID 6342Acetonitrile용매

실험 절차

2.4 g (0.0106 mol) of methyl 2-(2-hydroxyphenyl)-2-hydroxyimino-acetate (Example VII-1a from process step 3; HPLC: 17.1% E, log p=0.95; 68.9% Z, log p=1.68) in 60 ml of acetonitrile are heated under reflux with 1.08 g (0.011 mol) of potassiun bicarbonate and 1.55 g (0.0123 mol) of dimethyl sulphate for 10 hours. The reaction mixture is poured into water and extracted with diethyl ether, and the solvent is distilled off under reduced pressure. This gives 2.1 g of crude product which is chromatographed over silica gel using a mixture of 7 parts of n-hexane and 3 parts of acetone. This gives 1.6 g of product which, according to HPLC, contains 36.9% of methyl Z-2-(2-hydroxyphenyl)-2-methoxyimino-acetate of log p=2.39.

후처리

  1. extractionextracted with diethyl ether
  2. distillationthe solvent is distilled off under reduced pressure
  3. customThis gives 2.1 g of crude product which is chromatographed over silica gel using
  4. additiona mixture of 7 parts of n-hexane and 3 parts of acetone

출처 및 근거

ORD 기록
ord-e4e138586a8a48c4a2249bdd49f6d329
출처 데이터셋
uspto-grants-2003_12
특허 번호
US06660872B1

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