Dimethylformamide → HCID 15070275、化合物

HRID 1073025ノート

反応式

HRID 1073025 の反応式
[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

参加物

6

反応物 4

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

生成物 1

HCID 15070275HCID 15070275、化合物収率 83.9%

試薬・触媒・溶媒 1

HCID 962Water溶媒

反応条件

温度
100 °C

実験手順

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.

後処理

  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)

出典と根拠

ORDレコード
ord-93c1f599379a44d6846451f41d515ed7
出典データセット
uspto-grants-1990_11
特許番号
US04968340

反応ノート

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