Phosphoric Acid → HCID 57558445、化合物

HRID 1723971ノート

反応式

HRID 1723971 の反応式
[OH:1][C:2]1[CH:7]=[CH:6][CH:5]=[C:4]([OH:8])[C:3]=1[C:9](=[O:12])[CH2:10][CH3:11].OP(O)(O)=O.B(F)(F)F.CCOCC.[CH3:27][C:28](=[CH2:30])[CH3:29].[OH-].[NH4+]>ClCCl>[C:28]([O:1][C:2]1[CH:7]=[CH:6][CH:5]=[C:4]([OH:8])[C:3]=1[C:9](=[O:12])[CH2:10][CH3:11])([CH3:30])([CH3:29])[CH3:27]

参加物

7

反応物 5

HCID 1004Phosphoric AcidHCID 8000Boron trifluoride etherateHCID 8255IsobutyleneHCID 14923Ammonium HydroxideHCID 116223911-(2,6-Dihydroxyphenyl)-propan-1-one

生成物 1

HCID 57558445HCID 57558445、化合物

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

反応条件

温度
-75 °C

実験手順

To a 100 mL round bottom flask is added 2′,6′dihydroxypropiophenone (25 g, 0.15 mol) and to it is then added dichloromethane (50 mL). This is then cooled to −75° C. and then 2.6 mL of H3PO4 is added to it followed by 6.22 mL of boron trifluoride etherate and then isobutylene (125 mL). The reaction is then stirred at −75° C. for 1.5 hrs and then at room temperature overnight. The reaction mixture is then poured into a 2N ammonium hydroxide solution (200 mL) and extracted with dichloromethane. The organic layer is then washed with water and then with brine and dried over sodium sulfate and filtered. The crude residue obtained after concentration of the filtrate is purified by flash chromatography using silica gel (ethyl acetate:hexanes) to afford the above product.

後処理

  1. customat room temperature
  2. customovernight
  3. extractionextracted with dichloromethane
  4. washThe organic layer is then washed with water
  5. dry with materialwith brine and dried over sodium sulfate
  6. filtrationfiltered

出典と根拠

ORDレコード
ord-9d97ec942ecb43a2afbd6b809b1b3742
出典データセット
uspto-grants-2009_02
特許番号
US07485283B2

反応ノート

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