Phosphorus oxychloride → 2,5-Dimethoxy-4-methylbenzaldehyde

HRID 493193

반응식

HRID 493193 반응식
[CH3:1][O:2][C:3]1[CH:8]=[CH:7][C:6]([O:9][CH3:10])=[CH:5][C:4]=1[CH3:11].O=P(Cl)(Cl)Cl.CN(C1C=CC=CC=1)[CH:19]=[O:20]>>[CH3:10][O:9][C:6]1[CH:5]=[C:4]([CH3:11])[C:3]([O:2][CH3:1])=[CH:8][C:7]=1[CH:19]=[O:20]

참가 물질

4

반응물 3

HCID 24813Phosphorus oxychlorideHCID 66737N-MethylformanilideHCID 905522,5-Dimethoxytoluene

생성물 1

HCID 6020192,5-Dimethoxy-4-methylbenzaldehyde

실험 절차

To a solution of 2,5-dimethoxytoluene (4.66 g, 30.6 mmol) in 60 mL of N-methyl-N-phenyl-formamide was added at 0° C. POCl3 (8.41 mL, 3 eq.), and the mixture was heated for 60 Min. to 80° C. After cooling, the reaction mixture was poured onto crashed ice, twofold extracted with AcOEt, washed with water, dried over sodium sulfate, and evaporated to dryness. Flash chromatography (SiO2, hexane/AcOEt=9/1) afforded 4.153 g of the title compound as off-white solid.

후처리

  1. customto 80° C
  2. temperatureAfter cooling
  3. additionthe reaction mixture was poured
  4. extractiontwofold extracted with AcOEt
  5. washwashed with water
  6. dry with materialdried over sodium sulfate
  7. customevaporated to dryness

출처 및 근거

ORD 기록
ord-fd48ddd0fdfa42f486351990e9793359
출처 데이터셋
uspto-grants-2009_05
특허 번호
US07534788B2

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