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Ethyl Acetate → Tert-butyl 1-[3-(4-amidinophenyl)-2-oxo-5-oxazolidinylcarbonyl}piperid-4-yl-carboxylate

HRID 977212
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HRID 977212 반응식
O=C1O[N:5]=[C:4]([C:7]2[CH:12]=[CH:11][C:10]([N:13]3[CH2:17][CH:16]([C:18]([N:20]4[CH2:25][CH2:24][CH:23]([C:26]([O:28][C:29]([CH3:32])([CH3:31])[CH3:30])=[O:27])[CH2:22][CH2:21]4)=[O:19])[O:15][C:14]3=[O:33])=[CH:9][CH:8]=2)[NH:3]1.C(OCC)(=O)C>CO.[Ni]>[C:4]([C:7]1[CH:8]=[CH:9][C:10]([N:13]2[CH2:17][CH:16]([C:18]([N:20]3[CH2:21][CH2:22][CH:23]([C:26]([O:28][C:29]([CH3:31])([CH3:30])[CH3:32])=[O:27])[CH2:24][CH2:25]3)=[O:19])[O:15][C:14]2=[O:33])=[CH:11][CH:12]=1)(=[NH:3])[NH2:5]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 2

HCID 8857Ethyl AcetateHCID 136146332Tert-butyl 1-{3-[4-(5-oxo-1,2,4-oxadiazolin-3-yl)phenyl]-2-oxo-5-oxazolidinylcarbonyl}piperidine-4carboxylate

생성물 1

HCID 15340942Tert-butyl 1-[3-(4-amidinophenyl)-2-oxo-5-oxazolidinylcarbonyl}piperid-4-yl-carboxylate

시약·촉매·용매 2

HCID 935Nickel촉매HCID 887Methanol용매

실험 절차

1.37 g of tert-butyl 1-{3-[4-(5-oxo-1,2,4-oxadiazolin-3-yl)phenyl]-2-oxo-5-oxazolidinylcarbonyl}piperidine-4-carboxylate are dissolved in 50 ml of methanol and hydrogenated over Raney nickel. The reaction mixture is, subsequently filtered and the filtrate is concentrated in vacuo. The product obtained is treated with 20 ml of ethyl acetate, with heating, and the product, after cooling, is filtered off with suction. Tert-butyl 1-[3-(4-amidinophenyl)-2-oxo-5-oxazolidinylcarbonyl}piperid-4-yl-carboxylate is obtained, m.p. 160°.

후처리

  1. filtrationsubsequently filtered
  2. concentrationthe filtrate is concentrated in vacuo
  3. customThe product obtained
  4. temperaturewith heating
  5. temperaturethe product, after cooling
  6. filtrationis filtered off with suction

출처 및 근거

ORD 기록
ord-897d8cdcf67d4e078c37df591e1c2bb4
출처 데이터셋
uspto-grants-1997_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05614535

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