Water → 4-[3,4-Dimethoxy-2-(3-methoxy-2,2-dimethyl-propoxy)-phenyl]-indan-1-one

HRID 2171055ノート

反応式

HRID 2171055 の反応式
[OH:1][C:2]1[C:7]([O:8][CH3:9])=[C:6]([O:10][CH3:11])[CH:5]=[CH:4][C:3]=1[C:12]1[CH:20]=[CH:19][CH:18]=[C:17]2[C:13]=1[CH2:14][CH2:15][C:16]2=[O:21].Br[CH2:23][C:24]([CH3:29])([CH3:28])[CH2:25][O:26][CH3:27].C([O-])([O-])=O.[K+].[K+].O>CN(C=O)C>[CH3:9][O:8][C:7]1[C:2]([O:1][CH2:23][C:24]([CH3:29])([CH3:28])[CH2:25][O:26][CH3:27])=[C:3]([C:12]2[CH:20]=[CH:19][CH:18]=[C:17]3[C:13]=2[CH2:14][CH2:15][C:16]3=[O:21])[CH:4]=[CH:5][C:6]=1[O:10][CH3:11]

参加物

6

反応物 4

HCID 962WaterHCID 11430Potassium CarbonateHCID 649954481-Bromo-3-methoxy-2,2-dimethylpropaneHCID 674668064-(2-Hydroxy-3,4-dimethoxy-phenyl)-indan-1-one

生成物 1

HCID 674677154-[3,4-Dimethoxy-2-(3-methoxy-2,2-dimethyl-propoxy)-phenyl]-indan-1-one

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

反応条件

温度
100 °C

実験手順

Compound 303 (0.02 g, 0.07 mmol) and 1-bromo-3-methoxy-2,2-dimethyl-propane (0.12 g, 0.56 mmol) were dissolved in dry DMF (0.8 mL). K2CO3 (0.1 g, 0.68 mmol) were added. The suspension was heated at 100° C. for 18 h. H2O was added and the mixture was extracted with EtOAc (×2). The combined organic phases were washed with brine, dried (Na2SO4), filtered and concentrated. Purification by preparative HPLC afforded the title compound as an oil.

後処理

  1. extractionthe mixture was extracted with EtOAc (×2)
  2. washThe combined organic phases were washed with brine
  3. dry with materialdried (Na2SO4)
  4. filtrationfiltered
  5. concentrationconcentrated
  6. customPurification by preparative HPLC

出典と根拠

ORDレコード
ord-d03a410ef7f24d4cb26aafa49bfa414f
出典データセット
uspto-grants-2015_06
特許番号
US09051290B2

反応ノート

読み込み中…