p-Toluenesulfonic acid → HCID 10313396, 화합물

HRID 431551

반응식

HRID 431551 반응식
[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

참가 물질

4

반응물 2

HCID 6101p-Toluenesulfonic acidHCID 2752952-Chloro-4,5-diamino-6-methylpyrimidine2회

생성물 1

HCID 10313396HCID 10313396, 화합물수율 635.5%

시약·촉매·용매 1

HCID 6212Chloroform용매

반응 조건

온도
100 °C

실험 절차

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.

후처리

  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)

출처 및 근거

ORD 기록
ord-d8df764e92fc445eb202e2d7c9fe31da
출처 데이터셋
uspto-grants-2003_12
특허 번호
US06660745B1

연결된 노트

불러오는 중…