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Chloroform → HCID 20294030, 화합물

HRID 1413212
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HRID 1413212 반응식
[C:1]([NH:4][C:5]1[N:6]=[CH:7][S:8][CH:9]=1)(=[O:3])[CH3:2].[C:10]([O-])(=[O:12])[CH3:11].[Na+].C(Cl)(Cl)Cl>C(OC(=O)C)(=O)C.N1C=CC=CC=1>[C:1]([N:4]([C:10](=[O:12])[CH3:11])[C:5]1[N:6]=[CH:7][S:8][CH:9]=1)(=[O:3])[CH3:2]
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 3

HCID 6212ChloroformHCID 517045Sodium AcetateHCID 202940374-Acetamidothiazole

생성물 1

HCID 20294030HCID 20294030, 화합물

시약·촉매·용매 2

HCID 1049Pyridine용매HCID 7918Acetic Anhydride용매

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온도
100 °C

실험 절차

A solution of 4-acetylaminothiazole (2.85 g, 20 mM) in a mixture of acetic anhydride (30 ml) and pyridine (10 ml) was heated at 100° C. for 16 hours. The reaction mixture was cooled and poured onto an ice cold mixture of 20% aqueous sodium acetate (200 ml) and chloroform (200 ml.). The layers were separated the organic layer was washed with water, dried (MgSO4) and the solvents removed under vacuum to give an oil. Trituration with hexane followed by recrystallisation from di-isopropyl ether gave the title compound (1.8 g, 49%) m.p. 55° C. (Found: C, 45.8; H, 4.4; N, 15.5%. C7H8N2O2S requires: C, 45.6; H, 4.4; N, 15.2%)

후처리

  1. temperatureThe reaction mixture was cooled
  2. customThe layers were separated the organic layer
  3. washwas washed with water
  4. dry with materialdried (MgSO4)
  5. customthe solvents removed under vacuum
  6. customto give an oil
  7. customTrituration with hexane followed by recrystallisation from di-isopropyl ether

출처 및 근거

ORD 기록
ord-a01ee483548145f9a6d44e67dec6722f
출처 데이터셋
uspto-grants-1981_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04249012

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