Hydrochloric Acid → 4-(1,3-dipropyl-2,3,6,7-tetrahydro-2,6-dioxo-1H-purin-8-yl)benzenesulfonic acid potassium salt

HRID 1262527ノート

反応式

HRID 1262527 の反応式
[NH2:1][C:2]1[C:3](=[O:16])[N:4]([CH2:13][CH2:14][CH3:15])[C:5](=[O:12])[N:6]([CH2:9][CH2:10][CH3:11])[C:7]=1[NH2:8].[K+:17].[S:18]([C:22]1[CH:30]=[CH:29][C:25]([C:26]([O-])=O)=[CH:24][CH:23]=1)([OH:21])(=[O:20])=[O:19].[OH-].[K+].C(N=C=NCCCN(C)C)C.Cl.[OH-].[Na+]>O>[K+:17].[CH2:13]([N:4]1[C:3](=[O:16])[C:2]2[NH:1][C:26]([C:25]3[CH:24]=[CH:23][C:22]([S:18]([O-:21])(=[O:20])=[O:19])=[CH:30][CH:29]=3)=[N:8][C:7]=2[N:6]([CH2:9][CH2:10][CH3:11])[C:5]1=[O:12])[CH2:14][CH3:15]

参加物

8

反応物 6

HCID 313Hydrochloric AcidHCID 14797Potassium HydroxideHCID 14798Sodium HydroxideHCID 159081-Ethyl-3-(3'-dimethylaminopropyl)carbodiimideHCID 50986055,6-Diamino-1,3-dipropyl-2,4(1H,3H)-pyrimidinedioneHCID 23670833Potassium 4-carboxybenzenesulfonate

生成物 1

HCID 237027204-(1,3-dipropyl-2,3,6,7-tetrahydro-2,6-dioxo-1H-purin-8-yl)benzenesulfonic acid potassium salt収率 17%

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

A mixture of 5,6-diamino-1,3-dipropyl-2,4-(1H,3H)pyrimidinedione (16.0 g, 0.07 moles), 4-sulfobenzoic acid monopotassium salt (17.0 g, 0.0707 moles) and water (250 ml) is prepared, and the pH adjusted to 5.0 by the addition of 10% potassium hydroxide. To this solution is added ethyl-3-(3-dimethylaminopropyl)carbodiimide (13.6 g, 0.0707 moles) in one portion, and the pH maintained at 5.0±0.5 by the dropwise addition of 4 N hydrochloric acid. When the pH stabilizes, the reaction mixture is treated with sodium hydroxide (100 ml, 50%), boiled under reflux for ten minutes, treated with activated carbon, and filtered warm. The resulting solution is chilled in ice, treated with hydrochloric acid (12 N, 1350 ml), and filtered. The solids are dried, recrystallized from methanol, and dried at 78° to yield 5.12 grams of 4-(1,3-dipropyl-2,3,6,7-tetrahydro-2,6-dioxo-1H-purin-8-yl)benzenesulfonic acid potassium salt, mp greater than 360°.

後処理

  1. customis prepared
  2. temperatureunder reflux for ten minutes
  3. additiontreated with activated carbon
  4. filtrationfiltered
  5. temperaturewarm
  6. temperatureThe resulting solution is chilled in ice
  7. additiontreated with hydrochloric acid (12 N, 1350 ml)
  8. filtrationfiltered
  9. customThe solids are dried
  10. customrecrystallized from methanol
  11. customdried at 78°

出典と根拠

ORDレコード
ord-faa238c7a27a42e7abd425e4be929a7a
出典データセット
uspto-grants-1984_06
特許番号
US04452788

反応ノート

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