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

HRID 2171055노트

반응식

HRID 2171055 반응식
[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]

참가 물질

6

반응물 4

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

생성물 1

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

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

반응 조건

온도
100 °C

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-d03a410ef7f24d4cb26aafa49bfa414f
출처 데이터셋
uspto-grants-2015_06
특허 번호
US09051290B2

반응 노트

불러오는 중…