碘化钠 → HCID 14456867，化合物

HRID 279781笔记

反应方程式

HRID 279781 反应方程式
[CH3:1][O:2][C:3]1[CH:20]=[C:19]([O:21][CH3:22])[CH:18]=[CH:17][C:4]=1[CH2:5][N:6]1[CH:9]([CH2:10]OS(C)(=O)=O)[CH2:8][C:7]1=[O:16].[I-:23].[Na+]>CC(C)=O>[CH3:1][O:2][C:3]1[CH:20]=[C:19]([O:21][CH3:22])[CH:18]=[CH:17][C:4]=1[CH2:5][N:6]1[CH:9]([CH2:10][I:23])[CH2:8][C:7]1=[O:16]

参与物

4

反应物 2

HCID 5238碘化钠2 次HCID 13505934HCID 13505934，化合物

产物 1

HCID 14456867HCID 14456867，化合物收率 104.3%

试剂、催化剂与溶剂 1

HCID 180丙酮溶剂

实验过程

A mixture of 37.5 g (0.107 mole) of 1-(2,4-dimethoxy-benzyl)-4-(mesyloxymethyl)-2-azetidinone prepared according to the preceding paragraph, 250 ml of anhydrous acetone, and 56.3 g (0.376 mole) of sodium iodide is heated to boiling for 8 hours. To the mixture a further amount of 18.8 g (0.125 mole) of sodium iodide are added and the mixture is stirred for a further 8 hours under boiling. The mixture is evaporated to dryness on a water-bath (internal temperature 50° C.), the residue is rubbed with 100 ml of water and the oil thus obtained is extracted with 100 ml of dichloromethane. The aqueous layer is extracted three times with 50 ml of dichloromethane each. The united dichloromethane layers are dried over anhydrous magnesium sulfate, filtered and the filtrate is evaporated. Thus 40.3 g of 1-(2,4-dimethoxy-benzyl)-4-(iodomethyl)-2-azetidinone are obtained. Yield: 98%.

后处理

  1. customprepared
  2. temperatureis heated
  3. customThe mixture is evaporated to dryness on a water-bath (internal temperature 50° C.)
  4. customthe oil thus obtained
  5. extractionis extracted with 100 ml of dichloromethane
  6. extractionThe aqueous layer is extracted three times with 50 ml of dichloromethane each
  7. dry with materialThe united dichloromethane layers are dried over anhydrous magnesium sulfate
  8. filtrationfiltered
  9. customthe filtrate is evaporated

来源与证据

ORD记录
ord-b4e36deae4a942f78db7fcfcdd295c3f
来源数据集
uspto-grants-1986_05
专利号
US04587049

反应笔记

加载中…