Potassium Carbonate → tert-Butyl[4-(7-chloro-5-methylsulfanyloxazolo[5,4-d]pyrimidin-2-yl)-2,6-dimethylphenoxy]acetate

HRID 633616노트

반응식

HRID 633616 반응식
C(=O)([O-])[O-].[K+].[K+].[Cl:7][C:8]1[C:9]2[N:18]=[C:17]([C:19]3[CH:24]=[C:23]([CH3:25])[C:22]([OH:26])=[C:21]([CH3:27])[CH:20]=3)[O:16][C:10]=2[N:11]=[C:12]([S:14][CH3:15])[N:13]=1.Br[CH2:29][C:30]([O:32][C:33]([CH3:36])([CH3:35])[CH3:34])=[O:31]>CN(C)C=O>[Cl:7][C:8]1[C:9]2[N:18]=[C:17]([C:19]3[CH:24]=[C:23]([CH3:25])[C:22]([O:26][CH2:29][C:30]([O:32][C:33]([CH3:36])([CH3:35])[CH3:34])=[O:31])=[C:21]([CH3:27])[CH:20]=3)[O:16][C:10]=2[N:11]=[C:12]([S:14][CH3:15])[N:13]=1

참가 물질

5

반응 조건

온도
60 °C

실험 절차

7.46 g of potassium carbonate were added to a solution of 4.34 g of 4-(7-chloro-5-methylsulfanyloxazolo[5,4-d]pyrimidin-2-yl)-2,6-dimethylphenol in 45 ml of dimethylformamide, and 2.90 g of tert-butyl bromoacetate were then added. The mixture was stirred at 60° C. for 1 h. The cooled reaction mixture was then added to ice water, and the precipitated solid was filtered off with suction and washed with water. The solid was taken up in dichloromethane and dried over sodium sulfate, activated carbon was added and the mixture was filtered and concentrated under reduced pressure. This gave 4.20 g (71%) of the title compound, which was reacted further without any further purification.

후처리

  1. additionwere then added
  2. customThe cooled reaction mixture
  3. filtrationthe precipitated solid was filtered off with suction
  4. washwashed with water
  5. dry with materialdried over sodium sulfate, activated carbon
  6. additionwas added
  7. filtrationthe mixture was filtered
  8. concentrationconcentrated under reduced pressure
  9. customThis gave 4.20 g (71%) of the title compound, which was reacted further without any further purification

출처 및 근거

ORD 기록
ord-13169866d1014eb9a6548b35d9ea6f12
출처 데이터셋
uspto-grants-2016_04
특허 번호
US09321787B2

반응 노트

불러오는 중…