3,4-Dimethoxytoluene → 1,2-Dimethoxy-4-methyl-5-(2-cyano-3-methoxy-2-propenyl)benzene

HRID 26667

반응식

HRID 26667 반응식
[CH3:1][O:2][C:3]1[CH:4]=[C:5]([CH3:11])[CH:6]=[CH:7][C:8]=1[O:9][CH3:10].[CH3:12][O:13][CH:14](OC)[C:15](=[CH2:18])[C:16]#[N:17]>C(Cl)Cl>[CH3:10][O:9][C:8]1[CH:7]=[C:6]([CH2:18][C:15]([C:16]#[N:17])=[CH:14][O:13][CH3:12])[C:5]([CH3:11])=[CH:4][C:3]=1[O:2][CH3:1]

참가 물질

4

반응물 2

HCID 681263,4-DimethoxytolueneHCID 124234392-Dimethoxymethylacrylonitrile

생성물 1

HCID 544881951,2-Dimethoxy-4-methyl-5-(2-cyano-3-methoxy-2-propenyl)benzene

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

To a solution of 10 g. of 3,4-dimethoxytoluene and 9.6 g. of 2-dimethoxymethylacrylonitrile in 200 ml. of dry methylene chloride was added dropwise at 0°, 2.3 ml. (0.0197 mole) of stannic chloride. The reaction mixture was stirred for 6 hours at 20°-25°, diluted with 500 ml. of ether, and the resulting solution washed with a 5% sodium bicarbonate solution until the aqueous layer remained basic. The combined aqueous washings were backwashed with ether and the organic layers were then combined and dried (MgSO4). The solvent was then removed under reduced pressure leaving an off-white residue of crude 1,2-dimethoxy-4-methyl-5-(2-cyano-3-methoxy-2-propenyl)benzene.

후처리

  1. additiondiluted with 500 ml
  2. washof ether, and the resulting solution washed with a 5% sodium bicarbonate solution until the aqueous layer
  3. dry with materialdried (MgSO4)
  4. customThe solvent was then removed under reduced pressure

출처 및 근거

ORD 기록
ord-eaa1ae833ef0486bad04e17db3c6680f
출처 데이터셋
uspto-grants-1979_04
특허 번호
US04151196

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