Potassium Carbonate → Tert-butyl 4-vinylphenoxyacetate

HRID 1956735

反応式

HRID 1956735 の反応式
[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]

参加物

6

反応物 3

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

生成物 1

HCID 18762166Tert-butyl 4-vinylphenoxyacetate収率 93.2%

試薬・触媒・溶媒 2

HCID 4875Potassium Iodide触媒HCID 180Acetone溶媒

実験手順

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%).

後処理

  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

出典と根拠

ORDレコード
ord-dc4dc93b31724a8eba3b1e29793f6e5e
出典データセット
uspto-grants-1998_07
特許番号
US05780566

関連ノート

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