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Potassium Carbonate → HCID 57699826、化合物

HRID 1011039
ノート
印刷プレビュー

反応式

HRID 1011039 の反応式
FC(F)(F)C(O)=O.[CH3:8][CH:9]([O:11][CH2:12][CH2:13][O:14][C:15]1[N:23]=[C:22]2[C:18]([N:19]=[C:20]([O:24][CH3:25])[NH:21]2)=[C:17]([NH2:26])[N:16]=1)[CH3:10].C(=O)([O-])[O-].[K+].[K+].CS(O[CH2:38][CH:39]1[CH2:44][CH2:43][O:42][CH2:41][CH2:40]1)(=O)=O>CN(C)C=O.C(OCC)(=O)C>[CH3:10][CH:9]([O:11][CH2:12][CH2:13][O:14][C:15]1[N:23]=[C:22]2[C:18]([N:19]=[C:20]([O:24][CH3:25])[N:21]2[CH2:38][CH:39]2[CH2:44][CH2:43][O:42][CH2:41][CH2:40]2)=[C:17]([NH2:26])[N:16]=1)[CH3:8]
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

6

反応物 3

HCID 11430Potassium CarbonateHCID 15166436Oxan-4-ylmethyl methanesulfonateHCID 178493998HCID 178493998、化合物

生成物 1

HCID 57699826HCID 57699826、化合物収率 112.7%

試薬・触媒・溶媒 2

HCID 6228Dimethylformamide溶媒HCID 8857Ethyl Acetate
溶媒

反応条件

温度
60 °C

実験手順

To a solution of 2-({2-[(1-methylethyl)oxy]ethyl}oxy)-8-(methoxy)-9H-purin-6-amine trifluoroacetate salt (400 mg) in dry N,N-dimethylformamide (6.4 ml) was added potassium carbonate (579 mg). The reaction was stirred at 60° C. for 1.5 hours. The reaction was cooled and tetrahydro-2H-pyran-4-ylmethyl methanesulfonate (224 mg) was added. The reaction was stirred at 90° C. for 4 hours. The reaction was cooled and taken up in ethyl acetate and washed twice with water. The organic layer was separated, dried over magnesium sulphate, filtered and concentrated in vacuo to yield a yellow oil (432 mg). The product was purified by C18 reverse phase chromatography using water (containing 0.1% formic acid)-acetonitrile (containing 0.05% formic acid) as eluant (20-50%) to afford the title compound as a clear viscous oil (166 mg).

後処理

  1. temperatureThe reaction was cooled
  2. stirringThe reaction was stirred at 90° C. for 4 hours
  3. temperatureThe reaction was cooled
  4. washwashed twice with water
  5. customThe organic layer was separated
  6. dry with materialdried over magnesium sulphate
  7. filtrationfiltered
  8. concentrationconcentrated in vacuo

出典と根拠

ORDレコード
ord-f36145ade31a4edea4995b80fa408bfc
出典データセット
uspto-grants-2011_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07977344B2

反応ノート

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