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Potassium Carbonate → 2-Ethoxy-5-[1-[4-(4-methylphenoxy)phenoxy]-ethyl]-1,3,4-thiadiazole

HRID 3782
ノート
印刷プレビュー

反応式

HRID 3782 の反応式
[CH3:1][C:2]1[CH:15]=[CH:14][C:5]([O:6][C:7]2[CH:12]=[CH:11][C:10]([OH:13])=[CH:9][CH:8]=2)=[CH:4][CH:3]=1.C(=O)([O-])[O-].[K+].[K+].Br[CH:23]([C:25]1[S:26][C:27]([O:30][CH2:31][CH3:32])=[N:28][N:29]=1)[CH3:24]>CC(C)=O>[CH2:31]([O:30][C:27]1[S:26][C:25]([CH:23]([O:13][C:10]2[CH:11]=[CH:12][C:7]([O:6][C:5]3[CH:14]=[CH:15][C:2]([CH3:1])=[CH:3][CH:4]=3)=[CH:8][CH:9]=2)[CH3:24])=[N:29][N:28]=1)[CH3:32]
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 11430Potassium CarbonateHCID 6414404-(4-Methylphenoxy)phenolHCID 146523742-(1-Bromoethyl)-5-ethoxy-1,3,4-thiadiazole

生成物 1

HCID 142309302-Ethoxy-5-[1-[4-(4-methylphenoxy)phenoxy]-ethyl]-1,3,4-thiadiazole収率 73.6%

試薬・触媒・溶媒 1

HCID 180Acetone溶媒

実験手順

0.84 g of 4-(4-methylphenoxy)phenol was dissolved in 5 ml of acetone followed by adding 0.87 g of anhydrous potassium carbonate and 1.0 g of 2-(1-bromoethyl)-5-ethoxy-1,3,4-thiadiazole. The resulting mixture was refluxed with stirring and heating for 2 hours. After cooling, insoluble salts were filtered off, and acetone was distilled off under reduced pressure. The residue was purified by chromatography on silica gel to obtain 1.1 g of the compound No. 10 described in Table 1.

後処理

  1. temperatureThe resulting mixture was refluxed
  2. temperatureheating for 2 hours
  3. temperatureAfter cooling
  4. filtrationinsoluble salts were filtered off
  5. distillationacetone was distilled off under reduced pressure
  6. customThe residue was purified by chromatography on silica gel

出典と根拠

ORDレコード
ord-08f23e697a564844a42b9eee52f2f3d1
出典データセット
uspto-grants-1988_02
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04722934

反応ノート

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