氢化钠 → 喹螨醚

HRID 35836

反应方程式

HRID 35836 反应方程式
[H-].[Na+].[C:3]([C:7]1[CH:12]=[CH:11][C:10]([CH2:13][CH2:14][OH:15])=[CH:9][CH:8]=1)([CH3:6])([CH3:5])[CH3:4].Cl[C:17]1[C:26]2[C:21](=[CH:22][CH:23]=[CH:24][CH:25]=2)[N:20]=[CH:19][N:18]=1>CN(C=O)C.O>[C:3]([C:7]1[CH:8]=[CH:9][C:10]([CH2:13][CH2:14][O:15][C:17]2[C:26]3[C:21](=[CH:22][CH:23]=[CH:24][CH:25]=3)[N:20]=[CH:19][N:18]=2)=[CH:11][CH:12]=1)([CH3:6])([CH3:4])[CH3:5]

参与物

6

反应物 3

HCID 24758氢化钠HCID 788644-氯喹唑啉HCID 794104-叔丁基苯乙醇

产物 1

HCID 86356喹螨醚收率 28.4%

试剂、催化剂与溶剂 2

HCID 962聚[6-[4-(4-氰基苯基)苯氧基]己基甲基丙烯酸酯]溶剂HCID 6228N,N-二甲基甲酰胺溶剂2 次

实验过程

To a solution of 1.1 g of sodium hydride in 50 ml of DMF, 4.0 g of 2-[4-(t-butyl)phenyl]ethanol was added, and the mixture was stirred at room temperature for one hour. Then 3.6 g of 4-chloroquinazoline in 20 ml of DMF were added, and the mixture was stirred at room temperature overnight. The mixture was then poured into a mixture of ice in water. The product was extracted into CH2Cl2, and the resulting solution was concentrated to dryness. TLC showed one major spot and five minor spots. The product was purified by HPLC (silica gel, CH2Cl2). The fractions containing the major product were collected and concentrated, giving 1.9 g of the title product. Yield: 28.4%. M.P. 70°-71° C.

后处理

  1. stirringthe mixture was stirred at room temperature overnight
  2. extractionThe product was extracted into CH2Cl2
  3. concentrationthe resulting solution was concentrated to dryness
  4. customThe product was purified by HPLC (silica gel, CH2Cl2)
  5. additionThe fractions containing the major product
  6. customwere collected
  7. concentrationconcentrated

来源与证据

ORD记录
ord-378409998bb94c5480b3bbf142ebb392
来源数据集
uspto-grants-1995_05
专利号
US05411963

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