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Ethanol → HCID 19785347, 화합물

HRID 2248804
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HRID 2248804 반응식
[CH:1]1([NH:4][C:5]2[C:10]([NH:11][C:12]([NH:14][CH:15]3[CH2:20][CH2:19][N:18]([C:21]([O:23][CH2:24][CH3:25])=[O:22])[CH2:17][CH2:16]3)=S)=[CH:9][N:8]=[CH:7][N:6]=2)[CH2:3][CH2:2]1.C(O)C>[Hg]=O.CN(C)C(=O)C>[CH:1]1([N:4]2[C:12]([NH:14][CH:15]3[CH2:20][CH2:19][N:18]([C:21]([O:23][CH2:24][CH3:25])=[O:22])[CH2:17][CH2:16]3)=[N:11][C:10]3[C:5]2=[N:6][CH:7]=[N:8][CH:9]=3)[CH2:3][CH2:2]1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 2

HCID 702EthanolHCID 19785282HCID 19785282, 화합물

생성물 1

HCID 19785347HCID 19785347, 화합물수율 14.1%

시약·촉매·용매 2

HCID 30856Mercuric oxide촉매HCID 31374Dimethylacetamide용매

반응 조건

온도
80 °C

실험 절차

A mixture of 15.7 parts of ethyl 4-[[[[4-(cyclopropylamino)-5-pyrimidinyl]amino]thioxomethyl]amino]-1-piperidinecarboxylate, 20 parts of mercury(II) oxide, 40 parts of ethanol and 135 parts of N,N-dimethylacetamide was stirred overnight at 80° C. The reaction mixture was filtered over diatomaceous earth while hot. The filtrate was poured into water and the product was extracted with dichloromethane. The organic layer was dried, filtered and evaporated. The residue was crystallized from acetonitrile. The product was filtered off and dried, yielding 2.2 parts (14.1%) of ethyl 4-[(9-cyclopropyl-9H-purin-8-yl)amino]-1-piperidinecarboxylate; mp. 177.0° C. (compound 17).

후처리

  1. filtrationThe reaction mixture was filtered over diatomaceous earth while hot
  2. additionThe filtrate was poured into water
  3. extractionthe product was extracted with dichloromethane
  4. customThe organic layer was dried
  5. filtrationfiltered
  6. customevaporated
  7. customThe residue was crystallized from acetonitrile
  8. filtrationThe product was filtered off
  9. customdried

출처 및 근거

ORD 기록
ord-4d7d019a24bd449799d5156f83ca9c02
출처 데이터셋
uspto-grants-1991_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05041448

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