2-Bromoethanol → HCID 10084631, 화합물

HRID 1783307노트

반응식

HRID 1783307 반응식
Cl.[NH:2]1[CH2:7][CH2:6][CH:5]([C:8]2[C:17]3[C:12](=[CH:13][CH:14]=[CH:15][CH:16]=3)[C:11](=[O:18])[NH:10][CH:9]=2)[CH2:4][CH2:3]1.C(=O)([O-])[O-].[K+].[K+].Br[CH2:26][CH2:27][OH:28]>CC(=O)CC.O>[OH:28][CH2:27][CH2:26][N:2]1[CH2:7][CH2:6][CH:5]([C:8]2[C:17]3[C:12](=[CH:13][CH:14]=[CH:15][CH:16]=3)[C:11](=[O:18])[NH:10][CH:9]=2)[CH2:4][CH2:3]1

참가 물질

6

반응물 3

HCID 108982-BromoethanolHCID 11430Potassium CarbonateHCID 23084775HCID 23084775, 화합물

생성물 1

HCID 10084631HCID 10084631, 화합물수율 55.9%

시약·촉매·용매 2

HCID 962Water용매HCID 6569Methyl Ethyl Ketone용매

실험 절차

4-(Piperidin-4-yl)-2H-isoquinolin-1-one hydrochloride (0.8 g) obtained in Example 31, potassium carbonate (2.0 g) and 2-bromoethanol (1.88 g) were dissolved in 2-butanone and water (1 mL), and the mixture was heated under reflux for 4 hrs. After the completion of the reaction, the solvent was evaporated, and water was added to the obtained residue. The mixture was extracted with chloroform, the organic layer dried over magnesium sulfate. The solvent was evaporated, and the obtained residue was purified by silica gel column chromatography (chloroform:methanol=4:1+triethylamine 2%) to give 4-(1-(2-hydroxyethyl)piperidin-4-yl)-2H-isoquinolin-1-one (0.46 g) as white crystals.

후처리

  1. temperatureunder reflux for 4 hrs
  2. customAfter the completion of the reaction
  3. customthe solvent was evaporated
  4. additionwater was added to the obtained residue
  5. extractionThe mixture was extracted with chloroform
  6. dry with materialthe organic layer dried over magnesium sulfate
  7. customThe solvent was evaporated
  8. customthe obtained residue was purified by silica gel column chromatography (chloroform:methanol=4:1+triethylamine 2%)

출처 및 근거

ORD 기록
ord-7e7798d870ed40f6ba75e1445dc7f489
출처 데이터셋
uspto-grants-2009_03
특허 번호
US07501412B2

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