Sodium Hydroxide → 7-(5-Hydroxy-5-methylhexyl)-3-methylxanthine

HRID 1762535

反応式

HRID 1762535 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].[OH-].[Na+].Cl[CH2:16][CH2:17][CH2:18][CH2:19][C:20]([OH:23])([CH3:22])[CH3:21]>CN(C)C=O>[OH:23][C:20]([CH3:22])([CH3:21])[CH2:19][CH2:18][CH2:17][CH2:16][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 14798Sodium Hydroxide2 回HCID 706393-MethylxanthineHCID 137476791-Chloro-5-hydroxy-5-methylhexane

生成物 1

HCID 137476807-(5-Hydroxy-5-methylhexyl)-3-methylxanthine

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

反応条件

温度
110 °C

実験手順

83 g (0.5 mol) of 3-methylxanthine are dissolved in 500 ml of 1N sodium hydroxide solution (0.5 mol) under the influence of heat. The mixture is filtered, the water is distilled off under reduced pressure and the sodium salt which remains is dried under a high vacuum. After addition of 1.5 liters of dimethylformamide and 75.3 g (0.5 mol) of 1-chloro-5-hydroxy-5-methylhexane, the mixture is heated at 110° C. for 6 hours, while stirring, filtered hot and evaporated under reduced pressure, the residue obtained is taken up in 1 liter of hot 1N sodium hydroxide solution, the hot solution is filtered and, after cooling to room temperature, 6N hydrochloric acid is added dropwise, with stirring, until a pH of 9 is reached. The precipitate is filtered off with suction, washed neutral and dried in vacuo.

後処理

  1. temperatureof heat
  2. filtrationThe mixture is filtered
  3. distillationthe water is distilled off under reduced pressure
  4. dry with materialthe sodium salt which remains is dried under a high vacuum
  5. filtrationfiltered hot
  6. customevaporated under reduced pressure
  7. customthe residue obtained
  8. filtrationthe hot solution is filtered
  9. temperatureafter cooling to room temperature
  10. addition6N hydrochloric acid is added dropwise
  11. stirringwith stirring, until a pH of 9
  12. filtrationThe precipitate is filtered off with suction
  13. washwashed neutral
  14. customdried in vacuo

出典と根拠

ORDレコード
ord-bc9497aaf57043adbf80ce262f868ba1
出典データセット
uspto-grants-1989_05
特許番号
US04833146

関連ノート

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