Ethyl Acetate → HCID 178418534、化合物

HRID 3781

反応式

HRID 3781 の反応式
[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]

参加物

6

反応物 4

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

生成物 1

HCID 178418534HCID 178418534、化合物収率 74.2%

試薬・触媒・溶媒 1

HCID 180Acetone溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-f72db97d8ce54dbba8cafdb5ed72d91d
出典データセット
uspto-grants-1988_02
特許番号
US04722934

関連ノート

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