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4-Chlorobenzamide → 5-(4-Chlorophenyl)-1,3,4-oxathiazol-2-one

HRID 453088
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HRID 453088 반응식
[Cl:1][C:2]1[CH:10]=[CH:9][C:5]([C:6]([NH2:8])=[O:7])=[CH:4][CH:3]=1.Cl[C:12]([S:14]Cl)=[O:13]>C1(C)C=CC=CC=1>[Cl:1][C:2]1[CH:10]=[CH:9][C:5]([C:6]2[O:7][C:12](=[O:13])[S:14][N:8]=2)=[CH:4][CH:3]=1
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참가 물질

4

반응물 2

HCID 120844-ChlorobenzamideHCID 75990(Chlorothio)formyl chloride

생성물 1

HCID 8194535-(4-Chlorophenyl)-1,3,4-oxathiazol-2-one

시약·촉매·용매 1

HCID 1140Toluene용매

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온도
80 °C

실험 절차

To a solution of 4-chlorobenzamide (0.25 g, 1.60 mmol) in toluene (10 ml) was added chlorocarbonylsulfenyl chloride (0.70 ml, 8.03 mmol). The resulting reaction mixture was refluxed at 80° C. for 3 h. After the completion of the reaction (TLC monitoring), the mixture was concentrated, added diethyl ether and washed twice with water, twice with 5% NaHCO3, again with water, and was dried (Na2SO4), concentrated under vacuum to give the product (crude yield 0.520 g) that was carried forward to the next step without further purification.

후처리

  1. customThe resulting reaction mixture
  2. customAfter the completion of the reaction (TLC monitoring)
  3. concentrationthe mixture was concentrated
  4. additionadded diethyl ether
  5. washwashed twice with water, twice with 5% NaHCO3, again with water
  6. dry with materialwas dried (Na2SO4)
  7. concentrationconcentrated under vacuum
  8. customto give the product (crude yield 0.520 g) that
  9. customwas carried forward to the next step without further purification

출처 및 근거

ORD 기록
ord-0e5dd71bee76478889f029f9df9edabc
출처 데이터셋
uspto-grants-2013_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08492414B2

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