Sodium hydride → HCID 14720860、化合物

HRID 1463251ノート

反応式

HRID 1463251 の反応式
[Cl:1][C:2]1[N:7]=[C:6]([O:8][C:9]2[CH:14]=[CH:13][C:12]([OH:15])=[CH:11][CH:10]=2)[CH:5]=[CH:4][CH:3]=1.[H-].[Na+].Cl[CH2:19][N:20]1[C:24]([Cl:25])=[C:23]([Cl:26])[N:22]=[CH:21]1>CN(C)C=O>[Cl:1][C:2]1[N:7]=[C:6]([O:8][C:9]2[CH:14]=[CH:13][C:12]([O:15][CH2:19][N:20]3[C:24]([Cl:25])=[C:23]([Cl:26])[N:22]=[CH:21]3)=[CH:11][CH:10]=2)[CH:5]=[CH:4][CH:3]=1

参加物

5

反応物 3

HCID 24758Sodium hydrideHCID 144026921H-Imidazole, 4,5-dichloro-1-(chloromethyl)-HCID 146736064-(6-Chloro-2-pyridinyloxy)phenol

生成物 1

HCID 14720860HCID 14720860、化合物収率 80.6%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒3 回

反応条件

温度
50 °C

実験手順

At room temperature (about 20° C.), 4.9 g of 4-(6-chloro-2-pyridinyloxy)-phenol in 40 ml of anhydrous dimethylformamide is dripped into 0.6 g of 100% strength sodium hydride in 20 ml of anhydrous dimethylformamide. The mixture is subsequently stirred for 30 minutes at 50° C., and then 4.2 g of 1-chloromethyl-4,5-dichloroimidazole in 20 ml of anhydrous dimethylformamide is dripped in at room temperature. This mixture is stirred for 2 hours at 60° C. and overnight at room temperature. It is then stirred into 200 ml of ice water and the solution is extracted three times with methyl tert-butyl ether. The organic phase is washed with 5% strength sodium hydroxide solution and water, and dried, and the solvent is evaporated off under reduced pressure. The crude product obtained is recrystallized from toluene. There is obtained 6.6 g of 1-[4-(6-chloro-2-pyridinyloxy)-phenoxymethyl]-4,5-dichloroimidazole: m.p.: 94°-98° C.

後処理

  1. customAt room temperature
  2. customis dripped in at room temperature
  3. stirringThis mixture is stirred for 2 hours at 60° C. and overnight at room temperature
  4. extractionthe solution is extracted three times with methyl tert-butyl ether
  5. washThe organic phase is washed with 5% strength sodium hydroxide solution and water
  6. customdried
  7. customthe solvent is evaporated off under reduced pressure
  8. customThe crude product obtained
  9. customis recrystallized from toluene

出典と根拠

ORDレコード
ord-985d557c38384a658ebee42feecf573b
出典データセット
uspto-grants-1994_04
特許番号
US05300502

反応ノート

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