Formaldehyde → [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

反応式

HRID 6919 の反応式
[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

参加物

5

反応物 3

HCID 712FormaldehydeHCID 5049666Sodium triacetoxyborohydrideHCID 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

生成物 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

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-6f19733c657e4b04b7ed2ac578424390
出典データセット
uspto-grants-2006_08
特許番号
US07084145B2

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