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Sulfuryl chloride → HCID 19992468, 화합물

HRID 345504
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HRID 345504 반응식
[CH3:1][O:2][C:3](=[O:15])[CH2:4][CH2:5][C:6](=[O:14])[C:7]1[CH:12]=[CH:11][C:10]([Cl:13])=[CH:9][CH:8]=1.S(Cl)([Cl:19])(=O)=O>ClCCl>[Cl:19][CH:5]([C:6](=[O:14])[C:7]1[CH:8]=[CH:9][C:10]([Cl:13])=[CH:11][CH:12]=1)[CH2:4][C:3]([O:2][CH3:1])=[O:15]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 24648Sulfuryl chlorideHCID 230774Methyl 4-(4-chlorophenyl)-4-oxobutanoate

생성물 1

HCID 19992468HCID 19992468, 화합물

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

A solution of 179 g (0.79 mole) of methyl-3-(4-chlorobenzoyl)propionate in 175 mL of dichloromethane was cooled to 0° and treated dropwise with 69.8 mL (117.3 g; 0.86 mole, d=1.68) of sulfuryl chloride. After the addition was complete, the cold bath was removed, and the reaction mixture was allowed to warm to room temperature while stirring overnight. The mixture was treated with 100 mL of water and basified cautiously with 50% sodium hydroxide. The layers were separated, the dichloromethane layer dried over magnesium sulfate and evaporated under reduced pressure (245.3 g). The residue was purified by vacuum distillation (135° C./0.3 mm) to obtain three fractions for a total of 198.6 g (96%).

후처리

  1. additionAfter the addition
  2. customthe cold bath was removed
  3. additionThe mixture was treated with 100 mL of water and basified cautiously with 50% sodium hydroxide
  4. customThe layers were separated
  5. dry with materialthe dichloromethane layer dried over magnesium sulfate
  6. customevaporated under reduced pressure (245.3 g)
  7. distillationThe residue was purified by vacuum distillation (135° C./0.3 mm)
  8. customto obtain three fractions for a total of 198.6 g (96%)

출처 및 근거

ORD 기록
ord-0a9e9c142d6b4389bc168c3d76ca0624
출처 데이터셋
uspto-grants-1991_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05057534

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