Potassium Carbonate → Benzyl 5-(4,6-Dimethoxy-1,3,5-triazin-2-yl)oxy-2-methyl-3-methoxycarbonylbenzofuran-4-carboxylate

HRID 52001ノート

反応式

HRID 52001 の反応式
[OH:1][C:2]1[C:15]([C:16]([O:18][CH2:19][C:20]2[CH:25]=[CH:24][CH:23]=[CH:22][CH:21]=2)=[O:17])=[C:6]2[C:7]([C:11]([O:13][CH3:14])=[O:12])=[C:8]([CH3:10])[O:9][C:5]2=[CH:4][CH:3]=1.[CH3:26][O:27][C:28]1[N:33]=[C:32]([O:34][CH3:35])[N:31]=[C:30](S(C)(=O)=O)[N:29]=1.C(=O)([O-])[O-].[K+].[K+]>CN(C)C=O>[CH3:35][O:34][C:32]1[N:33]=[C:28]([O:27][CH3:26])[N:29]=[C:30]([O:1][C:2]2[C:15]([C:16]([O:18][CH2:19][C:20]3[CH:25]=[CH:24][CH:23]=[CH:22][CH:21]=3)=[O:17])=[C:6]3[C:7]([C:11]([O:13][CH3:14])=[O:12])=[C:8]([CH3:10])[O:9][C:5]3=[CH:4][CH:3]=2)[N:31]=1

参加物

5

反応物 3

HCID 11430Potassium CarbonateHCID 157900444,6-Dimethoxy-2-methylsulfonyl-1,3,5-triazineHCID 54269833Benzyl 5-hydroxy-2-methyl-3-methoxycarbonylbenzofuran-4-carboxylate

生成物 1

HCID 54466231Benzyl 5-(4,6-Dimethoxy-1,3,5-triazin-2-yl)oxy-2-methyl-3-methoxycarbonylbenzofuran-4-carboxylate収率 109.7%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

反応条件

温度
70 °C

実験手順

A mixture comprising 2 g of benzyl 5-hydroxy-2-methyl-3-methoxycarbonylbenzofuran-4-carboxylate, 1 g of 4,6-dimethoxy-2-methylsulfonyl-1,3,5-triazine and 1 g of potassium carbonate in 20 ml of N,N-dimethylformamide, was heated and stirred at 70° C. for two hours. The mixture was returned to room temperature, poured into ice water and extracted with ethyl acetate. The organic layer was washed with water and then dried over anhydrous sodium sulfate. Then, it was concentrated under reduced pressure, and the obtained solid was thoroughly washed with ethanol to obtain 2.4 g (yield: 86%) of the desired compound.

後処理

  1. temperaturewas heated
  2. customwas returned to room temperature
  3. extractionextracted with ethyl acetate
  4. washThe organic layer was washed with water
  5. dry with materialdried over anhydrous sodium sulfate
  6. concentrationThen, it was concentrated under reduced pressure
  7. washthe obtained solid was thoroughly washed with ethanol

出典と根拠

ORDレコード
ord-c8aeca6db46d47d69486361733e264f1
出典データセット
uspto-grants-1997_04
特許番号
US05616537

反応ノート

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