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Ethyl cyanoformate → HCID 12351253, 화합물

HRID 1963011
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HRID 1963011 반응식
[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([C:8]2OC(=O)[S:10][N:9]=2)=[CH:4][CH:3]=1.[C:14]([C:16]([O:18][CH2:19][CH3:20])=[O:17])#[N:15]>ClC1C=CC=CC=1Cl>[CH2:19]([O:18][C:16]([C:14]1[S:10][N:9]=[C:8]([C:5]2[CH:6]=[CH:7][C:2]([Cl:1])=[CH:3][CH:4]=2)[N:15]=1)=[O:17])[CH3:20]
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 69336Ethyl cyanoformateHCID 8194535-(4-Chlorophenyl)-1,3,4-oxathiazol-2-one

생성물 1

HCID 12351253HCID 12351253, 화합물수율 85%

시약·촉매·용매 1

HCID 72391,2-Dichlorobenzene용매

반응 조건

온도
150 °C

실험 절차

To a solution of 5-(4-chlorophenyl)-[1,3,4]oxathiazol-2-one (1.35 g, 6.32 mmol) in 1,2-dichlorobenzene (5 ml) was added ethyl cyanoformate (2.50 ml, 25.27 mmol). The resulting reaction mixture was refluxed for 24 h at 150° C. After the completion of the reaction (TLC monitoring), added ice-cold water and extracted with ethyl acetate (3×100 ml). The combined organic layer was dried over Na2SO4, filtered and concentrated under vacuum, to get the desired product (1.44 g, 85%).

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후처리

  1. customThe resulting reaction mixture
  2. customAfter the completion of the reaction (TLC monitoring)
  3. additionadded ice-cold water
  4. extractionextracted with ethyl acetate (3×100 ml)
  5. dry with materialThe combined organic layer was dried over Na2SO4
  6. filtrationfiltered
  7. concentrationconcentrated under vacuum

출처 및 근거

ORD 기록
ord-bb9a49f098a6472590d7db30409ff236
출처 데이터셋
uspto-grants-2013_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08415383B2

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