p-Toluenesulfonic acid → HCID 10313396、化合物

HRID 431551

反応式

HRID 431551 の反応式
[C:1]1(C)C=CC(S(O)(=O)=O)=C[CH:2]=1.[NH2:12][C:13]1[C:18]([NH2:19])=[C:17]([CH3:20])[N:16]=[C:15]([Cl:21])[N:14]=1>C(Cl)(Cl)Cl>[Cl:21][C:15]1[N:14]=[C:13]2[C:18]([NH:19][C:1]([CH3:2])=[N:12]2)=[C:17]([CH3:20])[N:16]=1

参加物

4

反応物 2

HCID 6101p-Toluenesulfonic acidHCID 2752952-Chloro-4,5-diamino-6-methylpyrimidine2 回

生成物 1

HCID 10313396HCID 10313396、化合物収率 635.5%

試薬・触媒・溶媒 1

HCID 6212Chloroform溶媒

反応条件

温度
100 °C

実験手順

After adding 10.1 ml of ortho-triethyl acetate, 0.23 g of para-toluenesulfonic acid and 73 ml of 2-methylpyrrolidone to 7.6 g of 4,5-diamino-2-chloro-6-methylpyrimidine, the mixture was heated at 100° C. and then heated and stirred while removing out of the system the ethanol produced during the reaction. After disappearance of the 4,5-diamino-2-chloro-6-methylpyrimidine, the reaction solution was further heated and stirred at 180° C. for 2 hours. After cooling to room temperature, chloroform was added thereto for dilution. The mixture solution was washed with water and then washed with saturated brine, after which the organic layer was dried over anhydrous magnesium sulfate and concentrated under reduced pressure. The residue was purified by silica gel column chromatography (chloroform:methanol=95:5) to obtain 1.55 g of the title compound.

後処理

  1. temperatureheated
  2. customwhile removing out of the system the ethanol
  3. customproduced during the reaction
  4. stirringstirred at 180° C. for 2 hours
  5. temperatureAfter cooling to room temperature
  6. washThe mixture solution was washed with water
  7. washwashed with saturated brine
  8. dry with materialafter which the organic layer was dried over anhydrous magnesium sulfate
  9. concentrationconcentrated under reduced pressure
  10. customThe residue was purified by silica gel column chromatography (chloroform:methanol=95:5)

出典と根拠

ORDレコード
ord-d8df764e92fc445eb202e2d7c9fe31da
出典データセット
uspto-grants-2003_12
特許番号
US06660745B1

関連ノート

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