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llms.txt · MCP 가이드개인정보처리방침 · 이용약관 · 지원v1.8.0
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Methanol → HCID 178507181, 화합물

HRID 1029381
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HRID 1029381 반응식
[C@@H:1]1([N:10]2[C:19]3[N:18]=[CH:17][N:16]=[C:14]([NH2:15])[C:13]=3[N:12]=[CH:11]2)[O:9][C@H:6]([CH2:7][OH:8])[C@@H:4]([OH:5])[C@H:2]1[OH:3].CO.ClC1C=C(C=CC=1)C(OO)=[O:27]>C(OCC)(=O)C>[C@@H:1]1([N:10]2[C:19]3[C:13](=[C:14]([N+:16]([O-:27])=[CH:17][N:18]=3)[NH2:15])[N:12]=[CH:11]2)[O:9][C@H:6]([CH2:7][OH:8])[C@@H:4]([OH:5])[C@H:2]1[OH:3]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 887MethanolHCID 60961AdenosineHCID 70297m-Chloroperbenzoic acid3회

생성물 1

HCID 178507181HCID 178507181, 화합물

시약·촉매·용매 1

HCID 8857Ethyl Acetate용매

실험 절차

In a 1-L round-bottomed flask protected with a calcium sulfate drying tube was placed a 5.0 g (18.7 mmol) of adenosine and 500 mL of methanol. The mixture was stirred at room temperature and 4.85 g (22.5 mmol) of m-chloroperoxybenzoic acid (MCPBA) was added in 7-10 portions over 2 hours. If thin-layer chromatography after 15-20 hours of stirring indicates the presence of starting material an additional 0.5 g (2.9 mmol) of MCPBA should be added and the reaction stirred an additional 4 hours. If the TLC continues to show starting material another portion of MCPBA must be added and the stirring continued overnight. After the TLC showed little or no starting material left the reaction mixture was poured slowly in 2 L of ethyl acetate with good stirring. After having been stirred 2 hours, the product was collected, washed with ethyl acetate, and dried in vacuo over phosphorus pentoxide: yield 4.6 g. Melting point and elemental analysis data are set forth in Table I.

후처리

  1. customIn a 1-L round-bottomed flask protected with a calcium sulfate drying tube
  2. stirringIf thin-layer chromatography after 15-20 hours of stirring
  3. additionshould be added
  4. stirringthe reaction stirred an additional 4 hours
  5. additionmust be added
  6. customthe stirring continued overnight
  7. waitno starting material left the reaction mixture
  8. stirringAfter having been stirred 2 hours
  9. customthe product was collected
  10. washwashed with ethyl acetate
  11. dry with materialdried in vacuo over phosphorus pentoxide

출처 및 근거

ORD 기록
ord-11d4964238224a9cacc2d57b7ded39f9
출처 데이터셋
uspto-grants-1992_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05102873

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