氢化钠 → 2-n-butyl-1-(2-chloro-6-fluorophenyl)methyl-1H-imidazole

HRID 36975笔记

反应方程式

HRID 36975 反应方程式
[CH2:1]([C:5]1[NH:6][CH:7]=[CH:8][N:9]=1)[CH2:2][CH2:3][CH3:4].[H-].[Na+].[Cl:12][C:13]1[CH:20]=[CH:19][CH:18]=[C:17]([F:21])[C:14]=1[CH2:15]Cl>CN(C)C=O>[CH2:1]([C:5]1[N:6]([CH2:15][C:14]2[C:17]([F:21])=[CH:18][CH:19]=[CH:20][C:13]=2[Cl:12])[CH:7]=[CH:8][N:9]=1)[CH2:2][CH2:3][CH3:4]

参与物

5

反应物 3

HCID 24758氢化钠HCID 1086752-氯-6-氟氯苄HCID 118153512-丁基咪唑

产物 1

HCID 199367742-n-butyl-1-(2-chloro-6-fluorophenyl)methyl-1H-imidazole

试剂、催化剂与溶剂 1

HCID 6228N,N-二甲基甲酰胺溶剂3 次

实验过程

A solution of 2-n-butylimidazole (3.75 g, 0.03 mol) in dry dimethylformamide (4 mL) was added to sodium hydride (0.95 g) in dimethylformamide (18 mL). After the gas evolution subsided, the mixture was stirred one hour under argon and 2-chloro-6-fluorobenzylchloride (5.5. g, 0.031 mol) in dimethylformamide (7 mL) was added to produce an exotherm. The mixture was stirred for 17 hours at ambient temperature, diluted with ice water and extracted with ethyl acetate. The washed, dried, concentrated organic layer provided 7.63 (94%) of the title compound whose NMR was consistent with the structure. This material was used without further purification.

后处理

  1. customto produce an exotherm
  2. stirringThe mixture was stirred for 17 hours at ambient temperature
  3. extractionextracted with ethyl acetate
  4. customThe washed, dried

来源与证据

ORD记录
ord-9704dfb188a04c0780cfdc54597ca94e
来源数据集
uspto-grants-1995_05
专利号
US05418250

反应笔记

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