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Triethylamine → HCID 70401066、化合物

HRID 2119123
ノート
印刷プレビュー

反応式

HRID 2119123 の反応式
[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
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

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

生成物 1

HCID 70401066HCID 70401066、化合物収率 42%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-3c68b8b8590541d2a70aad080e5b8f78
出典データセット
uspto-grants-1987_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04683223

反応ノート

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