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Adenine → HCID 67823190、化合物

HRID 1492471
ノート
印刷プレビュー

反応式

HRID 1492471 の反応式
[H-].[Na+].[N:3]1[C:11]([NH2:12])=[C:10]2[C:6]([N:7]=[CH:8][NH:9]2)=[N:5][CH:4]=1.[C:13]([O:21][CH2:22][C@@H:23]1[C@@H:29]([CH2:30][O:31][C:32](=[O:39])[C:33]2[CH:38]=[CH:37][CH:36]=[CH:35][CH:34]=2)[CH2:28][CH:27]2[CH:25]([O:26]2)[CH2:24]1)(=[O:20])[C:14]1[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=1.P([O-])([O-])([O-])=O>CN(C=O)C.CO>[C:32]([O:31][CH2:30][C@@H:29]1[C@@H:23]([CH2:22][O:21][C:13](=[O:20])[C:14]2[CH:15]=[CH:16][CH:17]=[CH:18][CH:19]=2)[CH2:24][C@@H:25]([N:7]2[CH:8]=[N:9][C:10]3[C:6]2=[N:5][CH:4]=[N:3][C:11]=3[NH2:12])[C@H:27]([OH:26])[CH2:28]1)(=[O:39])[C:33]1[CH:38]=[CH:37][CH:36]=[CH:35][CH:34]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

7

反応物 4

HCID 190AdenineHCID 1061PhosphateHCID 24758Sodium hydrideHCID 15280201HCID 15280201、化合物

生成物 1

HCID 67823190HCID 67823190、化合物収率 48%

試薬・触媒・溶媒 2

HCID 887Methanol溶媒
HCID 6228
Dimethylformamide
溶媒

実験手順

In an atmosphere of argon gas, 60% sodium hydride (20 mg, 0.65 mole) was added to a suspension of adenine (202.5 mg, 1.34 mmoles) in anhydrous DMF (10 ml). After stirring the mixture at room temperature for one hour, (3S,4S)-3,4-bis(benzoyloxymethyl)-7-oxabicyclo-[4.1.0]heptane (245 mg, 0.67 mmole) was added and the resulting mixture was heated in an oil bath kept at 140° C. for 3 hours. After adding 0.2M phosphate buffer (pH 7.0) to the reaction mixture and stirring the mixture for a while, the mixture was subjected to extraction with ethyl acetate. After drying the extract solution on anhydrous sodium sulfate, the solvent was distilled off under reduced pressure, and the residue was purified by silica gel column chromatography (methylene chloride:methanol=50:1, v/v) to obtain 9-[(1R,2R,4S,5S)-4,5-bis(benzoyloxymethyl)-2-hydroxycyclohexyl]-adenine (161 mg, Yield 48%).

後処理

  1. temperaturethe resulting mixture was heated in an oil bath
  2. waitkept at 140° C. for 3 hours
  3. stirringstirring the mixture for a while
  4. extractionthe mixture was subjected to extraction with ethyl acetate
  5. dry with materialAfter drying the extract solution on anhydrous sodium sulfate
  6. distillationthe solvent was distilled off under reduced pressure
  7. customthe residue was purified by silica gel column chromatography (methylene chloride

出典と根拠

ORDレコード
ord-73336e9fc4404977b11249c3cd543c26
出典データセット
uspto-grants-1994_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05374625

反応ノート

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