反応 #456839

ord-1991e42ff5074b4fbbab4d50391b7b85

反応方程式

CCc1cc(O)cc(CC)c1OCCCCOCC=C(Cl)Cl
3,5-diethyl-4-(4-(3,3-dichloro-2-propenyloxy)butyloxy)phenol
ClCC=C(Cl)Cl
1,1,3-trichloro-1-propene
O=C([O-])[O-].[K+].[K+]
potassium carbonate
CN(C)C=O
N,N-dimethylformamide
CCc1cc(OCC=C(Cl)Cl)cc(CC)c1OCCCCOCC=C(Cl)Cl
3,5-diethyl-1-(3,3-dichloro-2-propenyloxy)-4-(4-(3,3-dichloro-2-propenyloxy)butyloxy)benzene
収率 72.0%

溶媒

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    抽出extracted twice with 50 ml of diethyl ether
  2. 2
    洗浄washed with water
  3. 3
    乾燥dried over magnesium sulfate
  4. 4
    濃縮concentrated

実験手順

A reaction vessel was charged with 0.35 g of 3,5-diethyl-4-(4-(3,3-dichloro-2-propenyloxy)butyloxy)phenol, 0.16 g of 1,1,3-trichloro-1-propene, 0.15 g of potassium carbonate and 10 ml of N,N-dimethylformamide. After stirring at room temperature for 24 hours, the reaction mixture was poured into water and extracted twice with 50 ml of diethyl ether. The diethyl ether layers were combined, washed with water, dried over magnesium sulfate and then concentrated. The residue was subjected to silica gel chromatography, which afforded 0.33 g of 3,5-diethyl-1-(3,3-dichloro-2-propenyloxy)-4-(4-(3,3-dichloro-2-propenyloxy)butyloxy)benzene (yield, 72%), nD24.4 1.5311.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US06140274uspto-grants-2000_10