Benzaldehyde → Ethyl 2-(benzylideneamino)acetate

HRID 1263166

반응식

HRID 1263166 반응식
Cl.[NH2:2][CH2:3][C:4]([O:6][CH2:7][CH3:8])=[O:5].S([O-])([O-])(=O)=O.[Mg+2].C(N(CC)CC)C.[CH:22](=O)[C:23]1[CH:28]=[CH:27][CH:26]=[CH:25][CH:24]=1>C(Cl)Cl>[C:4]([CH2:3][N:2]=[CH:22][C:23]1[CH:28]=[CH:27][CH:26]=[CH:25][CH:24]=1)([O:6][CH2:7][CH3:8])=[O:5]

참가 물질

6

반응물 4

HCID 240BenzaldehydeHCID 8471TriethylamineHCID 24083Sulfuric acid magnesium salt (1:1)HCID 2723640Glycine ethyl ester, hydrochloride

생성물 1

HCID 357745Ethyl 2-(benzylideneamino)acetate

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

To ethyl glycinate hydrochloride (36.4 g) suspended in 500 ml methylene chloride were added magnesium sulfate (22 g) and triethylamine (72 ml, 52.4 g). Benzaldehyde (27.6 g) was added dropwise at 15°-20° C. with stirring. The mixture was stirred at room temperature for two hours, filtered and stripped. To the residue was added 300 ml diethylether and 150 ml brine. After separation the organic layer was collected, and the aqueous layer was extracted with 100 ml ether. The organic phases were combined, dried (MgSO4), filtered and stripped to yield the title product as a pale yellow oil.

후처리

  1. stirringThe mixture was stirred at room temperature for two hours
  2. filtrationfiltered
  3. additionTo the residue was added 300 ml diethylether and 150 ml brine
  4. customAfter separation the organic layer
  5. customwas collected
  6. extractionthe aqueous layer was extracted with 100 ml ether
  7. dry with materialdried (MgSO4)
  8. filtrationfiltered

출처 및 근거

ORD 기록
ord-aa81e46f05784623b13d2ebc3b0c126b
출처 데이터셋
uspto-grants-1984_06
특허 번호
US04456467

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