Water → Ethyl Z-2-(2-acetamidothiazol-4-yl)-2-butenoate

HRID 2231370노트

반응식

HRID 2231370 반응식
[C:1]([NH:4][C:5]([NH2:7])=[S:6])(=[O:3])[CH3:2].O.[CH:9](=[C:11]([C:17](=O)[CH2:18]Cl)[C:12]([O:14][CH2:15][CH3:16])=[O:13])[CH3:10]>CN(C)C=O>[C:1]([NH:4][C:5]1[S:6][CH:10]=[C:9](/[C:11](=[CH:17]/[CH3:18])/[C:12]([O:14][CH2:15][CH3:16])=[O:13])[N:7]=1)(=[O:3])[CH3:2]

참가 물질

5

반응물 3

HCID 962WaterHCID 2723593AcetylthioureaHCID 54518096Ethyl 2-ethylidene-4-chloro-3-oxobutyrate

생성물 1

HCID 13603194Ethyl Z-2-(2-acetamidothiazol-4-yl)-2-butenoate

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

반응 조건

온도
15 °C

실험 절차

14.6 parts by weight of acetylthiourea, 30 parts by volume of water and 50 parts by volume of N,N-dimethylformamide are heated up to 85° C. under nitrogen. 22.9 parts by weight of ethyl 2-ethylidene-4-chloro-3-oxobutyrate are then added at this temperature in the course of 40 minutes. The mixture is stirred at 80° to 85° C. for 1 hour and then cooled to 15° C., and, after 10 minutes, the precipitate which has separated out is filtered off with suction. The precipitate is suspended once in 34.5 parts by volume of water, filtered off with suction again and washed twice more with water. The crude product is dried and then extracted by stirring once in a mixture of 13.8 parts by volume of water and 41.8 parts by volume of ethanol for 10 minutes, filtered off with suction and rinsed with ethanol/water (3/1). After drying, 8.8 parts by weight of a pure product are obtained.

후처리

  1. waitafter 10 minutes
  2. customthe precipitate which has separated out
  3. filtrationis filtered off with suction
  4. filtrationfiltered off with suction again
  5. washwashed twice more with water
  6. dry with materialThe crude product is dried
  7. extractionextracted
  8. stirringby stirring once in a mixture of 13.8 parts by volume of water and 41.8 parts by volume of ethanol for 10 minutes
  9. filtrationfiltered off with suction
  10. washrinsed with ethanol/water (3/1)
  11. customAfter drying
  12. custom8.8 parts by weight of a pure product are obtained

출처 및 근거

ORD 기록
ord-da6a6ce211b54166a06580024a2f263c
출처 데이터셋
uspto-grants-1988_11
특허 번호
US04782162

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