2-Bromoethanol → HCID 10084631、化合物

HRID 1783307ノート

反応式

HRID 1783307 の反応式
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

参加物

6

反応物 3

HCID 108982-BromoethanolHCID 11430Potassium CarbonateHCID 23084775HCID 23084775、化合物

生成物 1

HCID 10084631HCID 10084631、化合物収率 55.9%

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 6569Methyl Ethyl Ketone溶媒

実験手順

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.

後処理

  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%)

出典と根拠

ORDレコード
ord-7e7798d870ed40f6ba75e1445dc7f489
出典データセット
uspto-grants-2009_03
特許番号
US07501412B2

反応ノート

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