多聚甲醛 → [4-Benzyl-5-(3,4,5,6-tetrahydro-2H-[1,2']bipyridinyl-4-yl)-4H-[1,2,4]triazol-3-ylmethyl]-(2-methoxy-ethyl)-methyl-amine

HRID 6919

反应方程式

HRID 6919 反应方程式
[CH2:1]([N:8]1[C:12]([CH:13]2[CH2:18][CH2:17][N:16]([C:19]3[CH:24]=[CH:23][CH:22]=[CH:21][N:20]=3)[CH2:15][CH2:14]2)=[N:11][N:10]=[C:9]1[CH2:25][NH:26][CH2:27][CH2:28][O:29][CH3:30])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.C=O.[C:33](O[BH-](OC(=O)C)OC(=O)C)(=O)C.[Na+]>ClCCl>[CH2:1]([N:8]1[C:12]([CH:13]2[CH2:14][CH2:15][N:16]([C:19]3[CH:24]=[CH:23][CH:22]=[CH:21][N:20]=3)[CH2:17][CH2:18]2)=[N:11][N:10]=[C:9]1[CH2:25][N:26]([CH2:27][CH2:28][O:29][CH3:30])[CH3:33])[C:2]1[CH:3]=[CH:4][CH:5]=[CH:6][CH:7]=1

参与物

5

反应物 3

HCID 712多聚甲醛HCID 5049666三乙酰氧基硼氢化钠HCID 10409077[4-Benzyl-5-(3,4,5,6-tetrahydro-2H-[1,2']bipyridinyl-4-yl)-4H-[1,2,4]triazol-3-ylmethyl]-(2-methoxy-ethyl)-amine

产物 1

HCID 10432290[4-Benzyl-5-(3,4,5,6-tetrahydro-2H-[1,2']bipyridinyl-4-yl)-4H-[1,2,4]triazol-3-ylmethyl]-(2-methoxy-ethyl)-methyl-amine

试剂、催化剂与溶剂 1

HCID 6344二氯甲烷溶剂

实验过程

The amine from example 43 (50 mg, 0.12 mmol), formaldehyde (37% aq, 40 μl, 0.49 mmol) and sodium triacetoxyborohydride (51 mg, 0.24 mmol) in dichloromethane (1 ml) was stirred vigorously at room temperature for 21 hours. The reaction mixture was partitioned between dichloromethane and aqueous sodium carbonate solution, and the layers separated. The organic phase was dried (MgSO4), evaporated under reduced pressure, and the product triturated from ether to afford the title compound as a white solid.

后处理

  1. customThe reaction mixture was partitioned between dichloromethane and aqueous sodium carbonate solution
  2. customthe layers separated
  3. dry with materialThe organic phase was dried (MgSO4)
  4. customevaporated under reduced pressure
  5. customthe product triturated from ether

来源与证据

ORD记录
ord-6f19733c657e4b04b7ed2ac578424390
来源数据集
uspto-grants-2006_08
专利号
US07084145B2

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