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Dimethyl Sulfide → Methyl 2-chloro-6-formyl-benzoate

HRID 1476822
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HRID 1476822 반응식
[Cl:1][C:2]1[CH:11]=[CH:10][CH:9]=[C:8]([CH:12]=C)[C:3]=1[C:4]([O:6][CH3:7])=[O:5].[O:14]=[O+][O-].CSC>C(Cl)Cl>[Cl:1][C:2]1[CH:11]=[CH:10][CH:9]=[C:8]([CH:12]=[O:14])[C:3]=1[C:4]([O:6][CH3:7])=[O:5]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 1068Dimethyl SulfideHCID 24823OzoneHCID 90041379Methyl 2-chloro-6-vinylbenzoate

생성물 1

HCID 53408620Methyl 2-chloro-6-formyl-benzoate수율 56%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

Into a solution of methyl 2-chloro-6-vinylbenzoate (6.7 g, 34 mmol) in dry DCM (100 mL) was bubbled O3 at −78° C. over a 30 minute period. Next, nitrogen gas was bubbled into the solution until the solution was colorless. Dimethylsulfane (4.3 g, 68 mmol) was added dropwise and the resulting mixture was warmed to RT and stirred for 2 hours. The reaction mixture was subsequently washed with water (30 mL) and extracted with DCM (3×100 mL). The organic layers were combined, dried over Na2SO4, and concentrated. The crude product was purified by column chromatography eluting with a gradient of EtOAc (0-90%) and PE to give the title compound (3.8 g, 56%). 1H NMR (400 MHz, CDCl3) δ ppm 9.89 (s, 1H), 7.728 (d, J=7.2 Hz, 1H), 7.606 (d, J=8.0 Hz, 1H), 7.489 (t, J=8.0 Hz, 1H), 3.95 (s, 3H).

후처리

  1. customNext, nitrogen gas was bubbled into the solution until the solution
  2. washThe reaction mixture was subsequently washed with water (30 mL)
  3. extractionextracted with DCM (3×100 mL)
  4. dry with materialdried over Na2SO4
  5. concentrationconcentrated
  6. customThe crude product was purified by column chromatography
  7. washeluting with a gradient of EtOAc (0-90%) and PE

출처 및 근거

ORD 기록
ord-d34b14f058a442219c9753484aec3eba
출처 데이터셋
uspto-grants-2016_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09402841B2

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