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Triethylamine → HCID 70401066, 화합물

HRID 2119123
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HRID 2119123 반응식
[CH:1]1[N:6]=[C:5](Cl)[C:4]2[N:8]=[CH:9][N:10]([C@@H:11]3[O:15][C@H:14]([CH2:16][OH:17])[C@@H:13]([OH:18])[C@H:12]3[OH:19])[C:3]=2[N:2]=1.Cl.[CH3:21][O:22][C:23]1[CH:32]=[C:31]2[C:26]([CH2:27][CH:28]([NH2:33])[CH2:29][O:30]2)=[CH:25][CH:24]=1.C([N:36](CC)CC)C>C(O)C>[CH3:21][O:22][C:23]1[CH:32]=[C:31]2[C:26]([CH2:27][CH:28]([NH:33][NH:36][C:5]3[C:4]4[N:8]=[CH:9][N:10]([C:3]=4[N:2]=[CH:1][N:6]=3)[C@@H:11]3[O:15][C@H:14]([CH2:16][OH:17])[C@@H:13]([OH:18])[C@H:12]3[OH:19])[CH2:29][O:30]2)=[CH:25][CH:24]=1
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참가 물질

5

반응물 3

HCID 8471TriethylamineHCID 930036-Chloropurine ribosideHCID 30416007-Methoxy-3,4-dihydro-2H-1-benzopyran-3-amine--hydrogen chloride (1/1)

생성물 1

HCID 70401066HCID 70401066, 화합물수율 42%

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

A mixture of 0.56 g 6-chloropurine riboside, 0.5 g 7-methoxy-3-chromanylamine hydrochloride, and 0.48 g of triethylamine is refluxed in 25 ml ethanol under nitrogen for 20 hrs. Solvent is evaporated to dryness and residue is treated with cold water. The clear aqueous solution is decanted off, residue is dissolved in ethanol and volatiles are evaporated under vacuo. The crude solid is purified by flash-chromatography on silica-gel using 5% methanolchloroform as an eluant. Evaporation of solvent from pure fractions followed by crystallization from CHCl3 -hexane affords 0.35 g (42%) of N6 -[7-methoxy-3-chromanylamino]adenosine having a melting point of 205°-207° C.

후처리

  1. customSolvent is evaporated to dryness and residue
  2. additionis treated with cold water
  3. customThe clear aqueous solution is decanted off
  4. dissolutionresidue is dissolved in ethanol
  5. customvolatiles are evaporated under vacuo
  6. customThe crude solid is purified by flash-chromatography on silica-gel
  7. customEvaporation of solvent from pure fractions
  8. customfollowed by crystallization from CHCl3 -hexane

출처 및 근거

ORD 기록
ord-3c68b8b8590541d2a70aad080e5b8f78
출처 데이터셋
uspto-grants-1987_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04683223

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