2-Aminothiazole → HCID 14920282、化合物

HRID 918882ノート

反応式

HRID 918882 の反応式
CO[CH:3]=[C:4]([C:11]([O:13][CH3:14])=[O:12])[CH:5]=[CH:6][C:7]([O:9]C)=O.[NH2:15][C:16]1[S:17][CH:18]=[CH:19][N:20]=1>CN(C=O)C>[O:9]=[C:7]1[N:15]([C:16]2[S:17][CH:18]=[CH:19][N:20]=2)[CH:3]=[C:4]([C:11]([O:13][CH3:14])=[O:12])[CH:5]=[CH:6]1

参加物

4

反応物 2

HCID 21552-AminothiazoleHCID 71338068Dimethyl 4-(methoxymethylidene)pent-2-enedioate

生成物 1

HCID 14920282HCID 14920282、化合物収率 43%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

反応条件

温度
150 °C

実験手順

After 2 g (9.9 mmol) of dimethyl 4-(methoxymethylene)2-pentenedioate obtained in Example 1-1 was dissolved in 10 mL of DMF, 1 g (9.9 mmol) of 2-aminothiazole was added to the solution. Afterward, the resulting reaction solution was stirred under reflux at about 150° C. for 6 hours. After termination of the reaction was determined by liquid chromatography, the solvent was removed in vacuo and was then washed using brine, followed by drying using magnesium sulfate, and filtration. After distillation under reduced pressure, the resulting product was purified using column chromatography (hexane:ethylacetate=1:3) to obtain a target compound (Actual yield: 1 g, Percent yield: 43%).

後処理

  1. customAfterward, the resulting reaction solution
  2. customthe solvent was removed in vacuo
  3. washwas then washed
  4. customby drying
  5. filtrationmagnesium sulfate, and filtration
  6. distillationAfter distillation under reduced pressure
  7. customthe resulting product was purified
  8. customto obtain a target compound (Actual yield: 1 g, Percent yield: 43%)

出典と根拠

ORDレコード
ord-f38f9f6d475a4f5bae6ec4edbfe84b24
出典データセット
uspto-grants-2016_03
特許番号
US09271976B2

反応ノート

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