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Ethylmorpholine → L-Pyroglutamyl-L-alanine amide

HRID 972704
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HRID 972704 반응식
ClC1C(O[C:9](=[O:16])[C@@H:10]2[CH2:14][CH2:13][C:12](=[O:15])[NH:11]2)=C(Cl)C(Cl)=C(Cl)C=1Cl.Cl.[NH2:22][C@H:23]([C:25]([NH2:27])=[O:26])[CH3:24].C(N1CCOCC1)C>CN(C)C=O>[NH:11]1[C:12](=[O:15])[CH2:13][CH2:14][C@H:10]1[C:9]([NH:22][C@H:23]([C:25]([NH2:27])=[O:26])[CH3:24])=[O:16]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 7525EthylmorpholineHCID 2775816(S)-2-aminopropanamide hydrochlorideHCID 3035255Perchlorophenyl 5-oxo-L-prolinate

생성물 1

HCID 22799701L-Pyroglutamyl-L-alanine amide

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

3.75 g (10 mmols) of L-pyroglutamic acid pentachlorophenyl ester were stirred in 40 ml of dimethyl formamide with 1.5 g (12 mmols) of L-alanine amide hydrochloride and 1.54 ml (12 mmols) of N-ethylmorpholine for 4 hours. The solvent was distilled off in vacuo. The residue was dissolved in methanol and the solution was stirred successively with strongly basic and strongly acid ion exchangers. The exchanger was removed by filtration and concentration to dryness followed. The residue was triturated with ethyl acetate, dissolved in a little ethanol and precipitated with petroleum ether in the form of a resin that solidified under petroleum ether. Yield: 1.2 g, chromatographically unfirom without sharp melting point.

후처리

  1. distillationThe solvent was distilled off in vacuo
  2. dissolutionThe residue was dissolved in methanol
  3. customThe exchanger was removed by filtration and concentration to dryness
  4. customThe residue was triturated with ethyl acetate
  5. dissolutiondissolved in a little ethanol
  6. customprecipitated with petroleum ether in the form of a resin that

출처 및 근거

ORD 기록
ord-2f893fed8cbd42a69a1dfa7f1fd2bf65
출처 데이터셋
uspto-grants-1977_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04053588

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