Tetrahydrofuran → 5-(4-Methoxyphenyl)-1,3,4-oxathiazol-2-one

HRID 240810

반응식

HRID 240810 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[S:13]Cl.C1[CH2:19][O:18]CC1>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:19](=[O:18])[S:13][N:9]=2)=[CH:5][CH:4]=1

참가 물질

5

반응물 3

HCID 8028TetrahydrofuranHCID 25353Sulfur dichlorideHCID 769594-Methoxybenzamide

생성물 1

HCID 8194565-(4-Methoxyphenyl)-1,3,4-oxathiazol-2-one수율 88%

시약·촉매·용매 1

HCID 1140Toluene용매

반응 조건

온도
80 °C

실험 절차

4-Methoxybenzamide (3.0 g, 19.9 mmol) was suspended in a mixture of toluene (30 mL) and THF (15 mL), and chlorosulfenyl chloride (3.35 mL, 39.7 mmol) was then added to the suspension. The obtained mixture was stirred at 80° C. for 2.5 hours. The reaction solution was cooled to room temperature, and it was then concentrated under reduced pressure. Thereafter, diethyl ether was added to the residue, and insoluble materials were then removed by filtration, so as to obtain the title compound (3.64 g, 88%) in the form of a colorless solid.

후처리

  1. additionwas then added to the suspension
  2. temperatureThe reaction solution was cooled to room temperature
  3. concentrationit was then concentrated under reduced pressure
  4. additionThereafter, diethyl ether was added to the residue, and insoluble materials
  5. customwere then removed by filtration

출처 및 근거

ORD 기록
ord-a94f5d3b2c354ec1b946040e641dba93
출처 데이터셋
uspto-grants-2014_02
특허 번호
US08648103B2

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