Dichloromethane → 1-bromo-2-chloro-4-ethynylbenzene

HRID 1018810노트

반응식

HRID 1018810 반응식
[OH-].[Na+].Cl[C:4]([C:8]1[CH:13]=[CH:12][C:11]([Br:14])=[C:10]([Cl:15])[CH:9]=1)=[CH:5]C=O.ClCCl>O.O1CCOCC1>[Br:14][C:11]1[CH:12]=[CH:13][C:8]([C:4]#[CH:5])=[CH:9][C:10]=1[Cl:15]

참가 물질

6

반응물 3

HCID 6344DichloromethaneHCID 14798Sodium HydroxideHCID 57087279HCID 57087279, 화합물

생성물 1

HCID 223904241-bromo-2-chloro-4-ethynylbenzene

시약·촉매·용매 2

HCID 962Water용매HCID 312751,4-Dioxane용매2회

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온도
80 °C

실험 절차

40 g of sodium hydroxide are dissolved, under an inert atmosphere, in 230 ml of water, 120 ml of 1,4-dioxane are added and the reaction mixture is heated to 80° C. 17.5 g of 3-chloro-3-(4-bromo-3-chlorophenyl)propenal dissolved in 400 ml of 1,4-dioxane are added and the reaction mixture is stirred for 30 minutes at 80° C. The reaction mixture is allowed to cool to room temperature and 2300 ml of dichloromethane are then added. The phases are separated after settling has taken place and the organic phase is washed with water and dried over magnesium sulphate. The compound dissolved in a dichloromethane/1,4-dioxane mixture is used in its current form in the next step.

후처리

  1. additionare added
  2. temperatureto cool to room temperature
  3. customThe phases are separated after settling
  4. washthe organic phase is washed with water
  5. dry with materialdried over magnesium sulphate
  6. dissolutionThe compound dissolved in a dichloromethane/1,4-dioxane mixture

출처 및 근거

ORD 기록
ord-e9067f02cceb403792f678d8f0261533
출처 데이터셋
uspto-grants-2002_11
특허 번호
US06482986B1

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