Methane, dichloromethoxy- → 5-Chloro-2-methoxy-3-methylbenzaldehyde

HRID 2290537노트

반응식

HRID 2290537 반응식
[CH3:1][C:2]1[CH:7]=[C:6]([Cl:8])[CH:5]=[CH:4][C:3]=1[O:9]C.[CH3:11][O:12][CH:13](Cl)Cl>C(Cl)Cl.[Ti](Cl)(Cl)(Cl)Cl>[Cl:8][C:6]1[CH:7]=[C:2]([CH3:1])[C:13]([O:12][CH3:11])=[C:4]([CH:5]=1)[CH:3]=[O:9]

참가 물질

5

반응물 2

HCID 21004Methane, dichloromethoxy-HCID 767484-Chloro-2-methylanisole

생성물 1

HCID 133167535-Chloro-2-methoxy-3-methylbenzaldehyde

시약·촉매·용매 2

HCID 24193Titanium Tetrachloride촉매HCID 6344Dichloromethane용매

반응 조건

온도
0 °C

실험 절차

Titanium tetrachloride (21.6 g, 0.114 mole) was added to a solution of 2-methyl-4-chloroanisole (9 g, 0.057 mole) in methylene chloride at 0° C. Then, 1,1-dichloromethyl methyl ether (7.24 g, 0.063 mole) was added dropwise over a three minute period and the reaction mixture stirred at 0° C. for 30 minutes. The reaction was quenched by carefully pouring it into water (600 ml). The organic layer was separated and the aqueous phase extracted with methylene chloride (2×100 ml). The combined organic layer and extracts was washed with brine, dried (MgSO4) and concentrated under reduced pressure to a pale yellow solid (10.1 g).

후처리

  1. customThe reaction was quenched
  2. additionby carefully pouring it into water (600 ml)
  3. customThe organic layer was separated
  4. extractionthe aqueous phase extracted with methylene chloride (2×100 ml)
  5. washThe combined organic layer and extracts was washed with brine
  6. dry with materialdried (MgSO4)
  7. concentrationconcentrated under reduced pressure to a pale yellow solid (10.1 g)

출처 및 근거

ORD 기록
ord-d70ad4294ed1496f811f32daceee59ea
출처 데이터셋
uspto-grants-1986_10
특허 번호
US04617312

반응 노트

불러오는 중…