1-Bromo-3-chloropropane → HCID 66961254、化合物

HRID 68999

反応式

HRID 68999 の反応式
[C:1](=[O:4])([O-])[O-].[K+].[K+].[OH:7][C:8]1[CH:9]=[C:10]2[C:15](=[CH:16][CH:17]=1)[N:14]=[C:13](OC)[CH:12]=[CH:11]2.[Cl:20][CH2:21][CH2:22][CH2:23]Br>C(#N)C.O>[Cl:20][CH2:21][CH2:22][CH2:23][O:7][C:8]1[CH:9]=[C:10]2[C:15](=[CH:16][CH:17]=1)[N:14]([CH3:13])[C:1](=[O:4])[CH:12]=[CH:11]2

参加物

6

反応物 3

HCID 80061-Bromo-3-chloropropaneHCID 11430Potassium CarbonateHCID 450911926-Hydroxy-2-methoxyquinoline

生成物 1

HCID 66961254HCID 66961254、化合物

試薬・触媒・溶媒 2

HCID 962Water溶媒2 回HCID 6342Acetonitrile溶媒

実験手順

Potassium carbonate (0.829 g) was dissolved in acetonitrile (10 ml) and water (10 ml), and 6-hydroxy-2-methoxyquinoline (0.875 g) and 1-chloro-3-bromopropane (1.48 ml) was added thereto, and the mixture was stirred while heating under reflux for 4 hours. The reaction mixture was condensed under reduced pressure. Water was added to the residue, followed by extraction using ethyl acetate. The organic layer was dried with sodium sulfate, and was condensed under reduced pressure. The residue was purified by silica gel column chromatography (hexane:ethyl acetate=1:1). The purified product was condensed to dryness under reduced pressure to give the title compound (1.107 g) as a white powder.

後処理

  1. temperaturewhile heating
  2. temperatureunder reflux for 4 hours
  3. customcondensed under reduced pressure
  4. extractionfollowed by extraction
  5. dry with materialThe organic layer was dried with sodium sulfate
  6. customcondensed under reduced pressure
  7. customThe residue was purified by silica gel column chromatography (hexane:ethyl acetate=1:1)
  8. customcondensed to dryness under reduced pressure

出典と根拠

ORDレコード
ord-6af2b31558e94fa4a1dc4925a91fd34a
出典データセット
uspto-grants-2014_09
特許番号
US08822453B2

関連ノート

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