Chlorine → 2-Chlorohypoxanthine hydrochloride monohydrate

HRID 258072ノート

反応式

HRID 258072 の反応式
[Cl:1]Cl.[NH:3]1[C:12](=[O:13])[C:11]2[NH:10][CH:9]=[N:8][C:7]=2[NH:6][C:4]1=S>Cl>[OH2:13].[ClH:1].[Cl:1][C:4]1[NH:3][C:12](=[O:13])[C:11]2[NH:10][CH:9]=[N:8][C:7]=2[N:6]=1

参加物

4

反応物 2

HCID 24526ChlorineHCID 12681852-Thioxanthine

生成物 1

HCID 1355888212-Chlorohypoxanthine hydrochloride monohydrate

試薬・触媒・溶媒 1

HCID 313Hydrochloric Acid溶媒2 回

実験手順

230 g (3.24 mol) of chlorine are introduced into a suspension of 168.2 g (1.0 mol) of 2-thioxanthine in 68 liters of conc. hydrochloric acid in the course of about 5 hours at 3°-5° C. Then about 1 liter of hydrochloric acid is distilled off in a water jet vacuum, the residue is cooled to 0°to +5° C., suction filtered and washed with 0.5 liters of saturated, ice-cold brine and finally with 300 ml of isopropanol. After drying at 50° C. over a period of about 12 hours, 93 g (85.7% of theory) of colourless crystal powder are obtained. By preparing the free base and again converting it into the hydrochloride the title compound is obtained in analytically pure form. Elemental analysis corresponds to the composition C5H4Cl2N4O×H2O.

後処理

  1. distillationThen about 1 liter of hydrochloric acid is distilled off in a water jet vacuum
  2. temperaturethe residue is cooled to 0°to +5° C., suction
  3. filtrationfiltered
  4. washwashed with 0.5 liters of saturated, ice-cold brine
  5. customAfter drying at 50° C. over a period of about 12 hours
  6. custom93 g (85.7% of theory) of colourless crystal powder are obtained
  7. customBy preparing the free base

出典と根拠

ORDレコード
ord-0117ad3b6d334411bb69f8215464c5fc
出典データセット
uspto-grants-1993_11
特許番号
US05264573

反応ノート

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