Potassium Iodide → HCID 15571592、化合物

HRID 127931ノート

反応式

HRID 127931 の反応式
Cl.[NH2:2][C:3]1[N:8]=[C:7]([NH2:9])[C:6]([CH2:10][C:11]2[CH:16]=[CH:15][C:14]([O:17][CH3:18])=[C:13]([OH:19])[CH:12]=2)=[CH:5][N:4]=1.[C:20]([NH:23][C:24]1[CH:29]=[CH:28][C:27]([S:30][CH2:31][CH2:32][CH2:33]Cl)=[CH:26][CH:25]=1)(=[O:22])[CH3:21].[OH-].[K+].[I-].[K+]>CO>[NH2:2][C:3]1[N:8]=[C:7]([NH2:9])[C:6]([CH2:10][C:11]2[CH:16]=[CH:15][C:14]([O:17][CH3:18])=[C:13]([O:19][CH2:33][CH2:32][CH2:31][S:30][C:27]3[CH:28]=[CH:29][C:24]([NH:23][C:20](=[O:22])[CH3:21])=[CH:25][CH:26]=3)[CH:12]=2)=[CH:5][N:4]=1

参加物

6

反応物 4

HCID 4875Potassium IodideHCID 14797Potassium HydroxideHCID 14005891N-{4-[(3-Chloropropyl)sulfanyl]phenyl}acetamideHCID 15571588HCID 15571588、化合物

生成物 1

HCID 15571592HCID 15571592、化合物

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

A mixture of 3.6 g of 2,4-diamino-5-(3'-hydroxy-4'-methoxybenzyl)pyrimidine hydrochloride, 3.4 g of 3-(p-acetamidophenylthio)propyl chloride, 3.8 ml of methanol, 12 ml of an aqueous solution containing 0.027 mole of potassium hydroxide and 0.2 g of potassium iodide is heated at reflux for 20 hr. The mixture is cooled and filtered to remove a small amount of inorganic material. Water, (75 ml) is added to the filtrate, and the methanol is removed by vacuum distillation. After the addition of 50 ml of methylene chloride the mixture is stirred for 30 min. and then filtered to obtain a crystalline product. After twice recrystallizing from 50% aqueous ethanol the product 2,4-diamino-5-{3'-[3"-(p-acetamidophenylthio)propoxy]-4'-methoxybenzyl}pyrimidine, weighes 1.94 g and has m.p. 175°-177°.

後処理

  1. temperatureis heated
  2. temperatureat reflux for 20 hr
  3. temperatureThe mixture is cooled
  4. filtrationfiltered
  5. customto remove a small amount of inorganic material
  6. additionWater, (75 ml) is added to the filtrate
  7. customthe methanol is removed by vacuum distillation
  8. additionAfter the addition of 50 ml of methylene chloride the mixture
  9. filtrationfiltered
  10. customto obtain a crystalline product
  11. customAfter twice recrystallizing from 50% aqueous ethanol the product 2,4-diamino-5-{3'-[3"-(p-acetamidophenylthio)propoxy]-4'-methoxybenzyl}pyrimidine, weighes 1.94 g

出典と根拠

ORDレコード
ord-11226529870a4c3da0f0599f67bedf74
出典データセット
uspto-grants-1981_03
特許番号
US04258045

反応ノート

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