Potassium Carbonate → HCID 22007301、化合物

HRID 323856

反応式

HRID 323856 の反応式
C(=O)([O-])[O-].[K+].[K+].[CH2:7]([N:14]1[C:22]2[C:21](=[O:23])[NH:20][C:19](=[O:24])[N:18]([CH2:25][CH2:26][CH3:27])[C:17]=2[N:16]=[CH:15]1)[C:8]1[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=1.[CH2:28]([O:30][CH2:31]Cl)[CH3:29]>CN(C)C=O.O.CO>[CH2:7]([N:14]1[C:22]2[C:21](=[O:23])[N:20]([CH2:31][O:30][CH2:28][CH3:29])[C:19](=[O:24])[N:18]([CH2:25][CH2:26][CH3:27])[C:17]=2[N:16]=[CH:15]1)[C:8]1[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=1

参加物

7

反応物 3

HCID 11430Potassium CarbonateHCID 18523Chloromethyl ethyl ether2 回HCID 220073027-Benzyl-3-propylxanthine

生成物 1

HCID 22007301HCID 22007301、化合物

試薬・触媒・溶媒 3

HCID 887Methanol溶媒HCID 962Water溶媒2 回HCID 6228Dimethylformamide溶媒

反応条件

温度
60 °C

実験手順

1.71 g (12.0 mmol) of potassium carbonate were added to a hot solution of 2.2 g (7.7 mmol) of 7-benzyl-3-propylxanthine from stage a) in 60 ml of dimethylformamide at 60° C. and the mixture was stirred at 60° C. for 1 hour. 0.93 ml (10.0 mmol) of ethoxymethyl chloride was then added dropwise and the mixture was stirred at 80° C. for 4.5 hours. A further 0.5 ml (5.3 mmol) of ethoxymethyl chloride was then added and the mixture was again stirred for 6 hours. 12 ml of water and 5 ml of methanol were then added, the mixture was allowed to stand overnight, 60 ml of water were added again and the mixture was extracted three times using methyl tert-butyl ether. The combined organic phases were washed twice with water, dried using magnesium sulfate and concentrated under reduced pressure. The crude product was purified by flash chromatography on a silica gel column, dichloromethane/methanol (19.8/0.2).

後処理

  1. stirringthe mixture was stirred at 80° C. for 4.5 hours
  2. stirringthe mixture was again stirred for 6 hours
  3. waitto stand overnight
  4. extractionthe mixture was extracted three times
  5. washThe combined organic phases were washed twice with water
  6. customdried
  7. concentrationconcentrated under reduced pressure
  8. customThe crude product was purified by flash chromatography on a silica gel column, dichloromethane/methanol (19.8/0.2)

出典と根拠

ORDレコード
ord-fdfe6072ba324e2b8b4432b84f0efb8c
出典データセット
uspto-grants-2001_04
特許番号
US06214992B1

関連ノート

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