醋酸钠 → HCID 14452902，化合物

HRID 2165259笔记

反应方程式

HRID 2165259 反应方程式
[NH2:1][C:2]1[C:3]([Cl:11])=[N:4][C:5]([CH2:9][CH3:10])=[CH:6][C:7]=1[Cl:8].[C:12]([O-])(=[O:14])[CH3:13].[Na+]>C(OC(=O)C)(=O)C>[C:12]([NH:1][C:2]1[C:3]([Cl:11])=[N:4][C:5]([CH2:9][CH3:10])=[CH:6][C:7]=1[Cl:8])(=[O:14])[CH3:13]

参与物

4

反应物 2

HCID 517045醋酸钠HCID 14452901HCID 14452901，化合物

产物 1

HCID 14452902HCID 14452902，化合物

试剂、催化剂与溶剂 1

HCID 7918乙酐溶剂

实验过程

7.8 g (40.8 mmol) of 3-amino-2,4-dichloro-6-ethyl-pyridine are heated under reflux for two hours in a mixture of 40 ml of acetic anhydride and 4 g (49 mmol) of anhydrous sodium acetate. The mixture is subsequently evaporated in vacuo, the residue is partitioned between dilute NH3 solution and CHCl3, and the organic phase is separated off, dried using Na2SO4 and evaporated. The residue (11.2 g) consists of a mixture of mono- and diacetylated amine. It is dissolved in 50 ml of methanol, 10 g of powdered K2CO3 are added and the mixture is stirred for one hour at room temperature. It is subsequently evaporated and partitioned between water and CHCl3, and the organic phase is separated off and washed with 5% strength aqueous NaH2PO4 solution. After drying using Na2SO4, the organic phase is evaporated. The residue is stirred with ether and filtered off with suction. Yield 7.7 g (80.9% of theory) melting point: 142° C.

后处理

  1. customThe mixture is subsequently evaporated in vacuo
  2. customthe residue is partitioned between dilute NH3 solution and CHCl3
  3. customthe organic phase is separated off
  4. customdried
  5. customevaporated
  6. additionThe residue (11.2 g) consists of a mixture of mono- and diacetylated amine
  7. dissolutionIt is dissolved in 50 ml of methanol
  8. addition10 g of powdered K2CO3 are added
  9. customIt is subsequently evaporated
  10. custompartitioned between water and CHCl3
  11. customthe organic phase is separated off
  12. washwashed with 5% strength aqueous NaH2PO4 solution
  13. customAfter drying
  14. customthe organic phase is evaporated
  15. stirringThe residue is stirred with ether
  16. filtrationfiltered off with suction

来源与证据

ORD记录
ord-15bc2417e70f4dca9ca997e23f114d65
来源数据集
uspto-grants-1990_07
专利号
US04939262

反应笔记

加载中…