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Ethanol → Glycine, N-(m-nitrophenyl)-, ethyl ester

HRID 47720
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HRID 47720 반응식
[N+:1]([C:4]1[CH:5]=[C:6]([NH:10][CH2:11][C:12]([OH:14])=[O:13])[CH:7]=[CH:8][CH:9]=1)([O-:3])=[O:2].[CH2:15](O)[CH3:16]>O>[N+:1]([C:4]1[CH:5]=[C:6]([NH:10][CH2:11][C:12]([O:14][CH2:15][CH3:16])=[O:13])[CH:7]=[CH:8][CH:9]=1)([O-:3])=[O:2]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 702Ethanol2회HCID 25089Glycine, N-(m-nitrophenyl)-

생성물 1

HCID 19172Glycine, N-(m-nitrophenyl)-, ethyl ester

시약·촉매·용매 1

HCID 962Water용매

실험 절차

2 g of 3-nitrophenylglycine are heated for 20 hours with stirring at a temperature in the region of 100° C. in 100 cm3 of absolute ethanol containing 20 cm3 of 6.5N hydrochloric ethanol. The suspension is filtered at a temperature in the region of 50° C.; the filtrate is concentrated under reduced pressure (5 kPa) at a temperature in the region of 40° C. The residue obtained is taken up in water and then extracted with about 100 cm3 of ethyl acetate. The aqueous phase is made alkaline by addition of sodium carbonate until a pH in the region of 10 is obtained. The medium is extracted with ethyl acetate; the combined extracts are washed with aqueous sodium chloride solution, dried over magnesium sulfate and then concentrated under reduced pressure (5 kPa) at 40° C. 1 g of ethyl 3-nitrophenylglycinate is obtained in the form of a yellow oil. (Rf=0.38 in a 95/5 by volume mixture of dichloromethane/methanol, on a Merck 60F254R silica plate).

후처리

  1. filtrationThe suspension is filtered at a temperature in the region of 50° C.
  2. concentrationthe filtrate is concentrated under reduced pressure (5 kPa) at a temperature in the region of 40° C
  3. customThe residue obtained
  4. extractionextracted with about 100 cm3 of ethyl acetate
  5. additionby addition of sodium carbonate until a pH in the region of 10
  6. customis obtained
  7. extractionThe medium is extracted with ethyl acetate
  8. washthe combined extracts are washed with aqueous sodium chloride solution
  9. dry with materialdried over magnesium sulfate
  10. concentrationconcentrated under reduced pressure (5 kPa) at 40° C

출처 및 근거

ORD 기록
ord-bd901037b2d24274865054226e84c567
출처 데이터셋
uspto-grants-2004_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06699895B2

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