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

HRID 1700369노트

반응식

HRID 1700369 반응식
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

참가 물질

5

반응물 3

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

생성물 1

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

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-156ac2c7456a43eea2e0cedad0ca637f
출처 데이터셋
uspto-grants-2002_02
특허 번호
US06350757B1

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