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

HRID 544655노트

반응식

HRID 544655 반응식
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

참가 물질

6

반응물 4

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

생성물 1

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

시약·촉매·용매 1

HCID 8857Ethyl Acetate용매2회

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-dd213e223f904ea895d9f60ffebc329f
출처 데이터셋
uspto-grants-1984_05
특허 번호
US04451471

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