Ethyl Acetate → HCID 178418534, 화합물

HRID 3781

반응식

HRID 3781 반응식
[O:1]([C:8]1[CH:13]=[CH:12][C:11]([OH:14])=[CH:10][CH:9]=1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[C:15](=O)([O-])[O-].[K+].[K+].BrC[C:23]1[S:24][C:25]([O:28][CH2:29][CH3:30])=[N:26][N:27]=1.C(OCC)(=O)C>CC(C)=O>[CH2:29]([O:28][C:25]1[SH:24]([CH3:15])[C:23]([O:14][C:11]2[CH:10]=[CH:9][C:8]([O:1][C:2]3[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=3)=[CH:13][CH:12]=2)=[N:27][N:26]=1)[CH3:30]

참가 물질

6

반응물 4

HCID 8857Ethyl AcetateHCID 11430Potassium CarbonateHCID 132544-PhenoxyphenolHCID 201533922-Bromomethyl-5-ethoxy-1,3,4-thiadiazole

생성물 1

HCID 178418534HCID 178418534, 화합물수율 74.2%

시약·촉매·용매 1

HCID 180Acetone용매

실험 절차

0.76 g of 4-phenoxy phenol was dissolved in 10 ml of acetone followed by adding 0.6 g of anhydrous potassium carbonate and 1.0 g of 2-bromomethyl-5-ethoxy-1,3,4-thiadiazole. The resulting mixture was refluxed with stirring and heated for 2 hours. After cooling, 100 ml of ethyl acetate was added followed by washing with water for two times, and the resulting ethyl acetate layer was dried over anhydrous magnesium sulfate. Ethyl acetate was distilled over under reduced pressure, and the residue was purified by chromatography on silica gel to obtain 1.0 g of the compound No. 1 described in Table 1.

후처리

  1. temperatureThe resulting mixture was refluxed
  2. temperatureheated for 2 hours
  3. temperatureAfter cooling
  4. washby washing with water for two times
  5. dry with materialthe resulting ethyl acetate layer was dried over anhydrous magnesium sulfate
  6. distillationEthyl acetate was distilled over under reduced pressure
  7. customthe residue was purified by chromatography on silica gel

출처 및 근거

ORD 기록
ord-f72db97d8ce54dbba8cafdb5ed72d91d
출처 데이터셋
uspto-grants-1988_02
특허 번호
US04722934

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