Isopropanol → HCID 20195166、化合物
反応式
[Na].Cl[C:3]1[CH:8]=[C:7](Cl)[N:6]=[C:5]([C:10]2[CH:15]=[CH:14][C:13]([CH3:16])=[CH:12][CH:11]=2)[N:4]=1.[CH:17]([OH:20])([CH3:19])[CH3:18]>>[C:13]1([CH3:16])[CH:14]=[CH:15][C:10]([C:5]2[N:6]=[C:7]([O:20][CH:17]([CH3:19])[CH3:18])[CH:8]=[C:3]([O:20][CH:17]([CH3:19])[CH3:18])[N:4]=2)=[CH:11][CH:12]=1参加物
4
実験手順
21.16 g of sodium are dissolved in anhydrous isopropanol and to this solution are added 95.64 g of 4,6-dichloro-2-p-tolylpyrimidine at 60°-65° C. over 15 minutes. The mixture is then heated to the boil and refluxed for a further 4 hours to bring the reaction to completion. Excess isopropanol is then distilled off and the residual oil is taken up in chloroform. The chloroform layer is washed with water, dried over sodium sulfate, and filtered. The solvent is then distilled off, affording 112 g of 2-p-tolyl-4,6-bis-isopropoxypyrimidine in the form of a yellowish oil which is purified by high vacuum distillation. The boiling point is 123° C./5.332 Pascal.
後処理
- temperatureThe mixture is then heated to the boil
- temperaturerefluxed for a further 4 hours
- customthe reaction to completion
- distillationExcess isopropanol is then distilled off
- washThe chloroform layer is washed with water
- dry with materialdried over sodium sulfate
- filtrationfiltered
- distillationThe solvent is then distilled off
出典と根拠
- ORDレコード
- ord-e1ab474c78db4f5a86f686416ce0396d
- 出典データセット
- uspto-grants-1987_06
- 特許番号
- US04674229
反応ノート
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