Potassium Carbonate → Tert-butyl 4-vinylphenoxyacetate

HRID 343741

반응식

HRID 343741 반응식
[OH:1][C:2]1[CH:9]=[CH:8][C:5]([CH:6]=[CH2:7])=[CH:4][CH:3]=1.Br[CH2:11][C:12]([O:14][C:15]([CH3:18])([CH3:17])[CH3:16])=[O:13].C(=O)([O-])[O-].[K+].[K+]>CC(C)=O.[I-].[K+]>[CH:6]([C:5]1[CH:8]=[CH:9][C:2]([O:1][CH2:11][C:12]([O:14][C:15]([CH3:18])([CH3:17])[CH3:16])=[O:13])=[CH:3][CH:4]=1)=[CH2:7]

참가 물질

6

반응물 3

HCID 11430Potassium CarbonateHCID 624534-VinylphenolHCID 79177tert-Butyl bromoacetate

생성물 1

HCID 18762166Tert-butyl 4-vinylphenoxyacetate수율 93.2%

시약·촉매·용매 2

HCID 4875Potassium Iodide촉매HCID 180Acetone용매

실험 절차

In a 1500 ml sulfonation flask, 135.6 g (1.13 mol) of 4-hydroxystyrene and 220.2 g (1.13 mol) of tert-butyl bromoacetate are dissolved in 800 ml of acetone and to the solution are added 195.0 g (1.41 mol) of potassium carbonate and 0.8 g of potassium iodide. The resultant suspension is stirred for 4 hours at 60° C. bath temperature. After cooling, the inorganic salts are removed by filtration and the filtrate is concentrated. The oily residue is taken up in 1000 ml of diethyl ether, washed twice with 800 ml of 1.0N sodium hydroxide solution and then three times with 1000 ml of water. The organic phase is separated, dried over magnesium sulfate and concentrated, giving 246.5 g of the desired product as a clear oil (93.2 %).

후처리

  1. temperatureAfter cooling
  2. customthe inorganic salts are removed by filtration
  3. concentrationthe filtrate is concentrated
  4. washwashed twice with 800 ml of 1.0N sodium hydroxide solution
  5. customThe organic phase is separated
  6. dry with materialdried over magnesium sulfate
  7. concentrationconcentrated

출처 및 근거

ORD 기록
ord-d383a13cf04849398409b501a33df3de
출처 데이터셋
uspto-grants-1999_01
특허 번호
US05863701

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