Potassium Carbonate → 7-(5-Hydroxy-5-methyl-6-heptynyl)-3-methylxanthine

HRID 1738800ノート

反応式

HRID 1738800 の反応式
[CH3:1][N:2]1[C:10]2[N:9]=[CH:8][NH:7][C:6]=2[C:5](=[O:11])[NH:4][C:3]1=[O:12].Cl[CH2:14][CH2:15][CH2:16][CH2:17][C:18]([OH:22])([CH3:21])[C:19]#[CH:20].C(=O)([O-])[O-].[K+].[K+]>CN(C)C=O>[OH:22][C:18]([CH3:21])([C:19]#[CH:20])[CH2:17][CH2:16][CH2:15][CH2:14][N:7]1[C:6]2[C:5](=[O:11])[NH:4][C:3](=[O:12])[N:2]([CH3:1])[C:10]=2[N:9]=[CH:8]1

参加物

5

反応物 3

HCID 11430Potassium CarbonateHCID 706393-MethylxanthineHCID 131980541-Chloro-5-hydroxy-5-methyl-6-heptyne

生成物 1

HCID 218393427-(5-Hydroxy-5-methyl-6-heptynyl)-3-methylxanthine

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

33.2 g (0.2 mol) of 3-methylxanthine in 350 ml of dimethylformamide were stirred with 32.1 g (0.2 mol) of 1-chloro-5-hydroxy-5-methyl-6-heptyne from Example 1B1) in the presence of 13.8 g (0.1 mol) of potassium carbonate at 120° C. for 6 hours. The hot mixture was then filtered, evaporated to dryness under reduced pressure and taken up in ethanol and, at the boiling point, diisopropyl ether was added to cloudiness, and the mixture was left to crystallize with cooling.

後処理

  1. filtrationThe hot mixture was then filtered
  2. customevaporated to dryness under reduced pressure
  3. additionwas added to cloudiness
  4. waitthe mixture was left
  5. customto crystallize
  6. temperaturewith cooling

出典と根拠

ORDレコード
ord-e31cd4cb11704bedb52965070cc228db
出典データセット
uspto-grants-1999_10
特許番号
US05965555

反応ノート

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