(Chlorothio)formyl chloride → 5-(4-Methoxyphenyl)-1,3,4-oxathiazol-2-one

HRID 453089노트

반응식

HRID 453089 반응식
[CH3:1][O:2][C:3]1[CH:11]=[CH:10][C:6]([C:7]([NH2:9])=[O:8])=[CH:5][CH:4]=1.Cl[C:13]([S:15]Cl)=[O:14]>C1(C)C=CC=CC=1>[CH3:1][O:2][C:3]1[CH:11]=[CH:10][C:6]([C:7]2[O:8][C:13](=[O:14])[S:15][N:9]=2)=[CH:5][CH:4]=1

참가 물질

4

반응물 2

HCID 75990(Chlorothio)formyl chlorideHCID 769594-Methoxybenzamide

생성물 1

HCID 8194565-(4-Methoxyphenyl)-1,3,4-oxathiazol-2-one

시약·촉매·용매 1

HCID 1140Toluene용매

반응 조건

온도
80 °C

실험 절차

To a solution of 4-methoxybenzamide (0.30 g, 1.10 mmol) in toluene (10 ml) was added chlorocarbonylsulfenyl chloride (0.80 ml, 9.92 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 with twice with water, twice with 5% NaHCO3, again with water, and was dried (Na2SO4), concentrated under vacuum to give the product (crude yield 0.475 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 with twice with water
  6. dry with materialtwice with 5% NaHCO3, again with water, and was dried (Na2SO4)
  7. concentrationconcentrated under vacuum
  8. customto give the product (crude yield 0.475 g) that
  9. customwas carried forward to the next step without further purification

출처 및 근거

ORD 기록
ord-848742b7949449a7b4dacf7d6e2bf053
출처 데이터셋
uspto-grants-2013_07
특허 번호
US08492414B2

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