乙醇 → 2-(4-(1-Hydroxyethyl)phenyl)-5-decyloxypyrimidine

HRID 1938108

反应方程式

HRID 1938108 反应方程式
C(O)C.C(Cl)(Cl)Cl.[C:8]([C:11]1[CH:16]=[CH:15][C:14]([C:17]2[N:22]=[CH:21][C:20]([O:23][CH2:24][CH2:25][CH2:26][CH2:27][CH2:28][CH2:29][CH2:30][CH2:31][CH2:32][CH3:33])=[CH:19][N:18]=2)=[CH:13][CH:12]=1)(=[O:10])[CH3:9].[BH4-].[Na+]>O>[OH:10][CH:8]([C:11]1[CH:12]=[CH:13][C:14]([C:17]2[N:22]=[CH:21][C:20]([O:23][CH2:24][CH2:25][CH2:26][CH2:27][CH2:28][CH2:29][CH2:30][CH2:31][CH2:32][CH3:33])=[CH:19][N:18]=2)=[CH:15][CH:16]=1)[CH3:9]

参与物

6

反应物 4

HCID 702乙醇HCID 6212三氯甲烷HCID 4311764硼氢化钠HCID 196949012-(4-Acetylphenyl)-5-decyloxypyrimidine

产物 1

HCID 214682802-(4-(1-Hydroxyethyl)phenyl)-5-decyloxypyrimidine收率 99.9%

试剂、催化剂与溶剂 1

HCID 962聚[6-[4-(4-氰基苯基)苯氧基]己基甲基丙烯酸酯]溶剂

实验过程

To a mixed solvent of 200 ml of ethanol and 100 ml of chloroform were added 35.5 g (0.1 mole) of 2-(4-acetylphenyl)-5-decyloxypyrimidine, and while maintaining the temperature at 30° to 35° C., 2.65 g (0.07 mole) of sodium borohydride were gradually added thereto. After stirring at the same temperature for 4 hours, the reaction mixture was poured into 500 ml of water and extracted with 400 ml of ethyl acetate. The organic phase was washed sufficiently, dried over anhydrous magnesium sulfate, and then the solvent was distilled off under reduced pressure to obtain 35.6 g (yield: 99.9 %) of 2-{4-(1-hydroxyethyl)phenyl}-5-decyloxypyrimidine.

后处理

  1. temperaturewhile maintaining the temperature at 30° to 35° C.
  2. extractionextracted with 400 ml of ethyl acetate
  3. washThe organic phase was washed sufficiently
  4. dry with materialdried over anhydrous magnesium sulfate
  5. distillationthe solvent was distilled off under reduced pressure

来源与证据

ORD记录
ord-c9046b081e0f4cf0b15ce782fba6c387
来源数据集
uspto-grants-1997_12
专利号
US05693251

关联笔记

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