Ethyl Acetate → 1-(1,1-Dimethylethyl) hydrogen L-glutamate

HRID 1860284노트

반응식

HRID 1860284 반응식
[C:1]([O:5][C:6](=[O:24])[C@@H:7]([NH:13]C(OCC1C=CC=CC=1)=O)[CH2:8][CH2:9][C:10]([OH:12])=[O:11])([CH3:4])([CH3:3])[CH3:2].C(OCC)(=O)C>CO.[Pd]>[C:1]([O:5][C:6](=[O:24])[C@@H:7]([NH2:13])[CH2:8][CH2:9][C:10]([OH:12])=[O:11])([CH3:4])([CH3:2])[CH3:3]

참가 물질

5

반응물 2

HCID 8857Ethyl AcetateHCID 6994036Z-Glu-OtBu

생성물 1

HCID 1175051-(1,1-Dimethylethyl) hydrogen L-glutamate

시약·촉매·용매 2

HCID 23938Palladium촉매HCID 887Methanol용매

실험 절차

To a solution of 25.0 g (74.1 mmol) (S)-2-(benzyloxycarbonylamino)pentanedioic acid 1-tert.-butyl ester (prepared according to Liebigs Ann. Chem. 1961, 646, 127) in 500 ml dry methanol were added 2.5 g 10% Pd/C, and the mixture was stirred over night at room temperature under an atmosphere of hydrogen. The catalyst was removed by filtration through celite and the filtrate was concentrated under reduced pressure. The remaining solid title compound was purified by stirring with a small amount of ethanol, filtered with suction, and dried in vacuo. Another crop (1.7 g) was obtained after concentration of the mother liquid and stirring of the residue with ethyl acetate.

후처리

  1. customThe catalyst was removed by filtration through celite
  2. concentrationthe filtrate was concentrated under reduced pressure
  3. customThe remaining solid title compound was purified
  4. stirringby stirring with a small amount of ethanol
  5. filtrationfiltered with suction
  6. customdried in vacuo
  7. customAnother crop (1.7 g) was obtained after concentration of the mother liquid

출처 및 근거

ORD 기록
ord-71008cb35c0747dc90dab36f4ad8ab56
출처 데이터셋
uspto-grants-2003_03
특허 번호
US06528534B2

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