Water → 4-Chloro-6-(3-methylbut-1-oxy)-2-phenylpyrimidine

HRID 1742755

反応式

HRID 1742755 の反応式
Cl[C:2]1[CH:7]=[C:6]([Cl:8])[N:5]=[C:4]([C:9]2[CH:14]=[CH:13][CH:12]=[CH:11][CH:10]=2)[N:3]=1.[OH2:15]>CC(C)CCO>[Cl:8][C:6]1[N:5]=[C:4]([C:9]2[CH:14]=[CH:13][CH:12]=[CH:11][CH:10]=2)[N:3]=[C:2]([O:15][CH2:11][CH2:10][CH:9]([CH3:14])[CH3:4])[CH:7]=1

参加物

4

反応物 2

HCID 962WaterHCID 77338Fenclorim

生成物 1

HCID 190067994-Chloro-6-(3-methylbut-1-oxy)-2-phenylpyrimidine

試薬・触媒・溶媒 1

HCID 31260Isoamyl Alcohol溶媒2 回

反応条件

温度
25 °C

実験手順

The reaction is carried out under an argon protective-gas atmosphere. A solution of 6.7 g (60.5 mmol) of sodium t-amylate in 50 ml of 3-methylbutanol is added dropwise to a solution, cooled to 0° C., of 12.4 g of 4,6-dichloro-2-phenylpyrimidine in 50 ml of 3-methylbutanol. The reaction mixture is allowed to warm to 25° C. overnight. Thin-layer chromatography shows the absence of starting material. The reaction mixture is poured into 180 ml of water and extracted three times with 80 ml of ethyl acetate. Combined organic phases are washed with water, dried using MgSO4 and filtered. Removal of the solvent gives 14.6 g (96% of theory) of the title compound.

後処理

  1. extractionextracted three times with 80 ml of ethyl acetate
  2. washCombined organic phases are washed with water
  3. customdried
  4. filtrationfiltered
  5. customRemoval of the solvent

出典と根拠

ORDレコード
ord-4992921d69164201ae402c37e8c994ce
出典データセット
uspto-grants-1994_08
特許番号
US05340701

関連ノート

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