Water → HCID 13505933, 화합물

HRID 279776노트

반응식

HRID 279776 반응식
[CH2:1]([O:3][C:4]([C:6]1(C(OCC)=O)[CH2:9][C:8](=[O:10])[N:7]1[CH2:11][C:12]1[CH:17]=[CH:16][C:15]([O:18][CH3:19])=[CH:14][C:13]=1[O:20][CH3:21])=[O:5])[CH3:2].[Cl-].[Na+].O>CS(C)=O>[CH2:1]([O:3][C:4]([CH:6]1[CH2:9][C:8](=[O:10])[N:7]1[CH2:11][C:12]1[CH:17]=[CH:16][C:15]([O:18][CH3:19])=[CH:14][C:13]=1[O:20][CH3:21])=[O:5])[CH3:2]

참가 물질

5

반응물 3

HCID 962WaterHCID 5234Sodium Chloride2회HCID 13505928HCID 13505928, 화합물

생성물 1

HCID 13505933HCID 13505933, 화합물수율 90.2%

시약·촉매·용매 1

HCID 679Dimethyl Sulfoxide용매

실험 절차

A mixture of 66.2 g (0.18 mole) of diethyl[1-(2,4-dimethoxy-benzyl)-4-oxo-2,2-azetidine-dicarboxylate] prepared according to the preceding paragraph, 70 ml of dimethyl sulfoxide, 12.7 g (0.22 mole) of sodium chloride and 6.5 ml (0.36 mole) of water is stirred on an oil bath (temperature 170°-180° C. for 6 hours. The reaction mixture is poured into 500 ml of a saturated aqueous sodium chloride solution, extracted five times with 100 ml ethyl acetate each, the organic phase is dried over anhydrous magnesium sulfate, filtered and from the filtrate the ethyl acetate is distilled off. Thus 47.6 g of ethyl-[1-(2,4-dimethoxy-benzyl)-4-oxo-2-azetidine-carboxylate] are obtained. B.p.: 170°-176° C./0.15 Hgmm.

후처리

  1. customprepared
  2. extractionextracted five times with 100 ml ethyl acetate each, the organic phase
  3. dry with materialis dried over anhydrous magnesium sulfate
  4. filtrationfiltered and from the filtrate the ethyl acetate
  5. distillationis distilled off

출처 및 근거

ORD 기록
ord-86aea116717242f48f5b6611ddc0bf3e
출처 데이터셋
uspto-grants-1986_05
특허 번호
US04587049

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