Methyl iodide → Ethyl 1-(6-chloro-2-methyl-2,3,4,9-tetrahydro-1H-beta-carbolin-1-yl)cyclobutanecarboxylate Hydrochloride

HRID 1700369ノート

反応式

HRID 1700369 の反応式
CI.[C:3]([O-])(O)=O.[Na+].Cl.[Cl:9][C:10]1[CH:11]=[C:12]2[C:20](=[CH:21][CH:22]=1)[NH:19][C:18]1[CH:17]([C:23]3([C:27]([O:29][CH2:30][CH3:31])=[O:28])[CH2:26][CH2:25][CH2:24]3)[NH:16][CH2:15][CH2:14][C:13]2=1>C(O)C>[ClH:9].[Cl:9][C:10]1[CH:11]=[C:12]2[C:20](=[CH:21][CH:22]=1)[NH:19][C:18]1[CH:17]([C:23]3([C:27]([O:29][CH2:30][CH3:31])=[O:28])[CH2:24][CH2:25][CH2:26]3)[N:16]([CH3:3])[CH2:15][CH2:14][C:13]2=1

参加物

5

反応物 3

HCID 6328Methyl iodideHCID 516892Sodium BicarbonateHCID 18317933Ethyl 1-(6-chloro-2,3,4,9-tetrahydro-1H-beta-carbolin-1-yl)cyclobutanecarboxylate Hydrochloride

生成物 1

HCID 18317948Ethyl 1-(6-chloro-2-methyl-2,3,4,9-tetrahydro-1H-beta-carbolin-1-yl)cyclobutanecarboxylate Hydrochloride

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

0.3 ml of methyl iodide and 0.8 g of NaHCO3 are added to a solution of 1 g of the compound of Example 1 in 25 ml of ethanol. After reaction for 24 hours at ambient temperature, the reaction mixture is concentrated under reduced pressure and then the residue is taken up in a mixture of water and dichloromethane. After extraction, drying and filtration, the organic phase is concentrated under reduced pressure. Crystallisation from a solution of ethanol and ethereal hydrogen chloride enables the expected product to be obtained.

後処理

  1. customAfter reaction for 24 hours at ambient temperature
  2. concentrationthe reaction mixture is concentrated under reduced pressure
  3. additionthe residue is taken up in a mixture of water and dichloromethane
  4. extractionAfter extraction
  5. customdrying
  6. filtrationfiltration
  7. concentrationthe organic phase is concentrated under reduced pressure
  8. customCrystallisation from a solution of ethanol and ethereal hydrogen chloride
  9. customto be obtained

出典と根拠

ORDレコード
ord-156ac2c7456a43eea2e0cedad0ca637f
出典データセット
uspto-grants-2002_02
特許番号
US06350757B1

反応ノート

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