Carbonic acid sodium salt (1:2) → HCID 58994150，化合物

HRID 12733

反应方程式

HRID 12733 反应方程式
[CH3:1][O:2][C:3]1[N:8]=[C:7]([O:9][CH3:10])[C:6](B(O)O)=[CH:5][N:4]=1.[CH3:14][C:15]1[CH:20]=[CH:19][N:18]=[CH:17][C:16]=1Br.C([O-])([O-])=O.[Na+].[Na+].C1C=CC(P(C2C=CC=CC=2)C2C=CC=CC=2)=CC=1>C(O)CC.CC([O-])=O.CC([O-])=O.[Pd+2]>[CH3:14][C:15]1[CH:20]=[CH:19][N:18]=[CH:17][C:16]=1[C:6]1[C:7]([O:9][CH3:10])=[N:8][C:3]([O:2][CH3:1])=[N:4][CH:5]=1

参与物

7

反应物 4

HCID 10340Carbonic acid sodium salt (1:2)HCID 11776三苯基膦HCID 8176304-甲基-3-溴吡啶HCID 27362092,4-二甲氧基嘧啶-5-硼酸

产物 1

HCID 58994150HCID 58994150，化合物

试剂、催化剂与溶剂 2

HCID 167845palladium acetate催化剂HCID 1031正丙醇溶剂

实验过程

2,4-Dimethoxypyrimidine-5-boronic acid (1.3 g, 7.23 mmol) was dissolved in degassed n-PrOH (20 ml) and then 4-methyl-3-bromo-pyridine (830 g, 4.82 mmol), Na2CO3 (1.02 g, 9.64 mmol), PPh3 (126 mg, 0.48 mmol) and Pd(OAc)2 (40 mg) were added. The suspension was stirred at reflux for 3 hours. The solvent was evaporated under vacuum and the crude was partitioned between water and DCM. The organic phase was dried (Na2SO4) and evaporated to give the title compound that was used without further purification in the next step (quantitative yield).

后处理

  1. temperatureat reflux for 3 hours
  2. customThe solvent was evaporated under vacuum
  3. customthe crude was partitioned between water and DCM
  4. dry with materialThe organic phase was dried (Na2SO4)
  5. customevaporated

来源与证据

ORD记录
ord-a66b7a3b045043e6b8987f76f458da43
来源数据集
uspto-grants-2010_06
专利号
US07727988B2

关联笔记

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