Ethanol → 5-Methoxy-2-(4-hydroxyphenyl)pyrimidine

HRID 485990ノート

反応式

HRID 485990 の反応式
[H][H].Cl[C:4]1[C:9]([O:10][CH3:11])=[C:8](Cl)[N:7]=[C:6]([C:13]2[CH:18]=[CH:17][C:16]([O:19]CC3C=CC=CC=3)=[CH:15][CH:14]=2)[N:5]=1.C(N(CC)CC)C.C(O)C>[Pd].O>[CH3:11][O:10][C:9]1[CH:8]=[N:7][C:6]([C:13]2[CH:18]=[CH:17][C:16]([OH:19])=[CH:15][CH:14]=2)=[N:5][CH:4]=1

参加物

7

反応物 4

HCID 702EthanolHCID 8471TriethylamineHCID 190970644,6-Dichloro-5-methoxy-2-(4-benzyloxyphenyl)pyrimidineHCID 178418361HCID 178418361、化合物

生成物 1

HCID 1357369415-Methoxy-2-(4-hydroxyphenyl)pyrimidine収率 90.9%

試薬・触媒・溶媒 2

HCID 23938Palladium触媒HCID 962Water溶媒

反応条件

温度
40 °C

実験手順

Hydrogen gas was blown into a mixture of 21 g of 4,6-dichloro-5-methoxy-2-(4-benzyloxyphenyl)pyrimidine, 18.1 g of triethylamine, 3.15 g of 10% palladium-on-carbon, 210 ml of ethanol, and 11 ml of water, followed by stirring at 40° C. for 6 hours. The catalyst was removed by filtration, and the filtrate was poured into 300 ml of water and extracted with ethyl acetate. The extract was dried over anhydrous sodium sulfate and distilled to remove ethyl acetate to afford 8.93 g (percent yield: 90.9%) of 5-methoxy-2-(4-hydroxyphenyl)pyrimidine.

後処理

  1. customThe catalyst was removed by filtration
  2. additionthe filtrate was poured into 300 ml of water
  3. extractionextracted with ethyl acetate
  4. dry with materialThe extract was dried over anhydrous sodium sulfate
  5. distillationdistilled
  6. customto remove ethyl acetate

出典と根拠

ORDレコード
ord-0bc80f25355f44b59294d2258f89aebc
出典データセット
uspto-grants-1994_03
特許番号
US05290477

反応ノート

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