Dimethylformamide → N,N-dimethyl 2-(4-chlorophenyl)-2-[(1,2,4-triazol-1-yl)methyl]-hexanamide

HRID 257733

反応式

HRID 257733 の反応式
[H-].[Na+].[Cl:3][C:4]1[CH:9]=[CH:8][C:7]([C:10]([CH2:18][N:19]2[CH:23]=[N:22][CH:21]=[N:20]2)([CH2:14][CH2:15][CH2:16][CH3:17])C(N)=O)=[CH:6][CH:5]=1.[CH3:24][N:25]([CH3:28])[CH:26]=[O:27]>>[CH3:24][N:25]([CH3:28])[C:26](=[O:27])[C:10]([C:7]1[CH:8]=[CH:9][C:4]([Cl:3])=[CH:5][CH:6]=1)([CH2:18][N:19]1[CH:23]=[N:22][CH:21]=[N:20]1)[CH2:14][CH2:15][CH2:16][CH3:17]

参加物

4

反応物 3

HCID 6228Dimethylformamide2 回HCID 24758Sodium hydrideHCID 199569562-(4-Chlorophenyl)-2-[(1,2,4-triazol-1-yl)methyl]hexanamide

生成物 1

HCID 20085208N,N-dimethyl 2-(4-chlorophenyl)-2-[(1,2,4-triazol-1-yl)methyl]-hexanamide収率 45.1%

実験手順

To a 100 mL 3 neck flask stirring under nitrogen was charged 1.5 g (0.9375 mole) 60% sodium hydride (prewashed with hexanes) in 50 mL of dimethyl formamide. To the slurry was charged 3.83 g (0.0125 mole) of 2-(4-chlorophenyl)-2-[(1,2,4-triazol-1-yl)methyl]hexanamide in 50 mL of dimethyl formamide. The mixture was stirred at room temperature for 3 hours then quenched by adding 20 mL of water and 75 mL of ether. The ether was washed with 50 mL water and the aqueous phase was extracted with 50 ml ethyl acetate. The ether was dried and concentrated and gave 1.88 g (45.1% yield) of product as an oil, Example 160 of Table 1.

後処理

  1. customthen quenched
  2. additionby adding 20 mL of water and 75 mL of ether
  3. washThe ether was washed with 50 mL water
  4. extractionthe aqueous phase was extracted with 50 ml ethyl acetate
  5. dry with materialThe ether was dried
  6. concentrationconcentrated

出典と根拠

ORDレコード
ord-e499b1e1b3ff402c89419ebaf7537efe
出典データセット
uspto-grants-1993_11
特許番号
US05264415

関連ノート

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