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Ethyl Acetate → HCID 14720869、化合物

HRID 654435
ノート
印刷プレビュー

反応式

HRID 654435 の反応式
[CH3:1][C:2]1[C:3]([O:9][C:10]2[CH:15]=[CH:14][C:13]([OH:16])=[CH:12][CH:11]=2)=[N:4][C:5]([CH3:8])=[CH:6][N:7]=1.[H-].[Na+].Cl[CH2:20][N:21]1[C:25]([Cl:26])=[C:24]([Cl:27])[N:23]=[CH:22]1.C(OCC)(=O)C>CN(C)C=O>[CH3:1][C:2]1[C:3]([O:9][C:10]2[CH:15]=[CH:14][C:13]([O:16][CH2:20][N:21]3[C:25]([Cl:26])=[C:24]([Cl:27])[N:23]=[CH:22]3)=[CH:12][CH:11]=2)=[N:4][C:5]([CH3:8])=[CH:6][N:7]=1
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 8857Ethyl AcetateHCID 24758Sodium hydrideHCID 144026921H-Imidazole, 4,5-dichloro-1-(chloromethyl)-HCID 199376084-(3,6-Dimethyl-2-pyrazinyloxy)-phenol

生成物 1

HCID 14720869HCID 14720869、化合物収率 67.6%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide
溶媒
3 回

反応条件

温度
70 °C

実験手順

At room temperature (about 20° C.), 7.8 g of 4-(3,6-dimethyl-2-pyrazinyloxy)-phenol in 20 ml of anhydrous dimethylformamide is dripped into 1.3 g of 80% strength sodium hydride in 30 ml of anhydrous dimethylformamide. The mixture is stirred for one hour at 70° C., and then 6.68 g of 1-chloromethyl-4,5-dichloroimidazole in 30 ml of anhydrous dimethylformamide is dripped in. The mixture is stirred for 8 hours at 70° C. and overnight at room temperature. It is then stirred into 200 ml of ethyl acetate, and this mixture is washed twice with water, four times with 5% strength sodium hydroxide solution and twice with saturated sodium chloride solution. The organic phase is dried over magnesium sulfate and the solvent is evaporated off under reduced pressure. The crude product obtained is crystallized with n-hexane. There is obtained 8.9 g of 1-[4-(3,6-dimethyl-2-pyrazinyloxy)-phenoxymethyl]-4,5-dichloroimidazole; m.p.: 84°-85° C.

後処理

  1. customAt room temperature
  2. stirringThe mixture is stirred for 8 hours at 70° C. and overnight at room temperature
  3. washthis mixture is washed twice with water, four times with 5% strength sodium hydroxide solution and twice with saturated sodium chloride solution
  4. dry with materialThe organic phase is dried over magnesium sulfate
  5. customthe solvent is evaporated off under reduced pressure
  6. customThe crude product obtained
  7. customis crystallized with n-hexane

出典と根拠

ORDレコード
ord-7d6b2d99b8b340bc917fec93306e9804
出典データセット
uspto-grants-1992_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05132308

反応ノート

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このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート