Dimethylformamide → HCID 15070275, 화합물

HRID 1073025

반응식

HRID 1073025 반응식
[OH:1][CH:2]([C:7]([CH3:10])([CH3:9])[CH3:8])[C:3]([O:5][CH3:6])=[O:4].[CH3:11][C:12]1[CH:17]=[C:16]([CH3:18])[N:15]=[C:14](S(C)(=O)=O)[N:13]=1.C(=O)([O-])[O-].[K+].[K+].CN(C)C=O>O>[CH3:11][C:12]1[CH:17]=[C:16]([CH3:18])[N:15]=[C:14]([O:1][CH:2]([C:7]([CH3:10])([CH3:9])[CH3:8])[C:3]([O:5][CH3:6])=[O:4])[N:13]=1

참가 물질

6

반응물 4

HCID 6228DimethylformamideHCID 11430Potassium CarbonateHCID 27723824,6-Dimethyl-2-methylsulfonylpyrimidineHCID 9855510Methyl 2-hydroxy-3,3-dimethylbutanoate

생성물 1

HCID 15070275HCID 15070275, 화합물수율 83.9%

시약·촉매·용매 1

HCID 962Water용매

반응 조건

온도
100 °C

실험 절차

2.9 g of methyl 2-hydroxy-3,3-dimethybutyrate, 4.1 g of 4,6 -dimethyl-2-methylsulfonylpyrimidine and 3.3 g of potassium carbonate were added to 50 ml of N,N-dimethylformamide, and the mixture was stirred at 100° C. for 4 hours. The reaction solution was cooled to room temperature, poured into water and extracted with 100 ml of ethyl acetate. The organic layer was washed twice with a sodium chloride aqueous solution, dried over anhydrous sodium sulfate and concentrated under reduced pressure. The liquid substance thereby obtained was purified by silica gel column chromatography (eluent: hexane/ethyl acetate =6/1) to obtain 4.2 g of the desired product.

후처리

  1. temperatureThe reaction solution was cooled to room temperature
  2. extractionextracted with 100 ml of ethyl acetate
  3. washThe organic layer was washed twice with a sodium chloride aqueous solution
  4. dry with materialdried over anhydrous sodium sulfate
  5. concentrationconcentrated under reduced pressure
  6. customThe liquid substance thereby obtained
  7. customwas purified by silica gel column chromatography (eluent: hexane/ethyl acetate =6/1)

출처 및 근거

ORD 기록
ord-93c1f599379a44d6846451f41d515ed7
출처 데이터셋
uspto-grants-1990_11
특허 번호
US04968340

연결된 노트

불러오는 중…