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Ethyl Acetate → HCID 14720869, 화합물

HRID 654435
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HRID 654435 반응식
[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
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

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

생성물 1

HCID 14720869HCID 14720869, 화합물수율 67.6%

시약·촉매·용매 1

HCID 6228Dimethylformamide
용매
3회

반응 조건

온도
70 °C

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-7d6b2d99b8b340bc917fec93306e9804
출처 데이터셋
uspto-grants-1992_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05132308

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