Acetic Acid → 2-[4,5-Bis-(p-methoxyphenyl)-thiazol-2-ylthio]-acetaldehyde

HRID 544655ノート

反応式

HRID 544655 の反応式
C[O:2][CH:3](OC)[CH2:4][S:5][C:6]1[S:7][C:8]([C:19]2[CH:24]=[CH:23][C:22]([O:25][CH3:26])=[CH:21][CH:20]=2)=[C:9]([C:11]2[CH:16]=[CH:15][C:14]([O:17][CH3:18])=[CH:13][CH:12]=2)[N:10]=1.C(O)(=O)C.S(=O)(=O)(O)O.O>C(OCC)(=O)C>[CH3:18][O:17][C:14]1[CH:15]=[CH:16][C:11]([C:9]2[N:10]=[C:6]([S:5][CH2:4][CH:3]=[O:2])[S:7][C:8]=2[C:19]2[CH:24]=[CH:23][C:22]([O:25][CH3:26])=[CH:21][CH:20]=2)=[CH:12][CH:13]=1

参加物

6

反応物 4

HCID 176Acetic AcidHCID 962WaterHCID 1118Sulfuric AcidHCID 132096712-[4,5-Bis-(p-methoxyphenyl)-thiazol-2-ylthio]-acetaldehyde-dimethylacetal

生成物 1

HCID 132096722-[4,5-Bis-(p-methoxyphenyl)-thiazol-2-ylthio]-acetaldehyde

試薬・触媒・溶媒 1

HCID 8857Ethyl Acetate溶媒2 回

実験手順

7.0 g of 2-[4,5-bis-(p-methoxyphenyl)-thiazol-2-ylthio]-acetaldehyde-dimethylacetal are mixed with 50 ml of acetic acid, 25 ml of sulphuric acid and 25 ml of water, stirred vigorously for 30 minutes, and then stirred into 1000 ml of ice-water. The oil which separates is taken up in 200 ml of ethyl acetate. Shaking is carried out with a further 200 ml of ethyl acetate and the combined organic phases are washed with water and then twice with cold sodium bicarbonate solution, dried over magnesium sulphate and concentrated to dryness by evaporation. The crude product is crystallised with diethyl ether. 2-[4,5-bis-(p-methoxyphenyl)-thiazol-2-ylthio]-acetaldehyde having a melting point of 75°-76° is obtained.

後処理

  1. stirringShaking
  2. washthe combined organic phases are washed with water
  3. dry with materialtwice with cold sodium bicarbonate solution, dried over magnesium sulphate
  4. concentrationconcentrated to dryness by evaporation
  5. customThe crude product is crystallised with diethyl ether

出典と根拠

ORDレコード
ord-dd213e223f904ea895d9f60ffebc329f
出典データセット
uspto-grants-1984_05
特許番号
US04451471

反応ノート

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