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

HRID 1476822
ノート
印刷プレビュー

反応式

HRID 1476822 の反応式
[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]
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

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

生成物 1

HCID 53408620Methyl 2-chloro-6-formyl-benzoate収率 56%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

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).

後処理

  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

出典と根拠

ORDレコード
ord-d34b14f058a442219c9753484aec3eba
出典データセット
uspto-grants-2016_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09402841B2

反応ノート

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