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Ethyl cyanoformate → HCID 12351253, 화합물

HRID 453091
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HRID 453091 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]>CCCCCCCCCCCC>[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 30.6%

시약·촉매·용매 1

HCID 8182Dodecane용매

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온도
150 °C

실험 절차

To a solution of 5-(4-chlorophenyl)-[1,3,4]oxathiazol-2-one (0.60 g, 2.80 mmol) in n-dodecane (0.80 ml) was added ethyl cyanoformate (1.10 ml, 11.20 mmol). The resulting reaction mixture was refluxed for 20 h at 150° C. After the completion of the reaction (TLC monitoring), added ice-cold water and extracted with ethyl acetate (3×75 ml). The combined organic layer was dried over Na2SO4, filtered and concentrated under vacuum. The crude residue was purified over silica gel (100-200 M, 20% EtOAc—Hexane) to get the product (0.23 g, 30%).

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 (3×75 ml)
  5. dry with materialThe combined organic layer was dried over Na2SO4
  6. filtrationfiltered
  7. concentrationconcentrated under vacuum
  8. customThe crude residue was purified over silica gel (100-200 M, 20% EtOAc—Hexane)

출처 및 근거

ORD 기록
ord-48a97d4577da42ad82688d254239c45b
출처 데이터셋
uspto-grants-2013_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08492414B2

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