Hydrochloric Acid → 7-Fluoro-2,3,4,9-tetrahydro-1H-beta-carboline

HRID 864480

반응식

HRID 864480 반응식
Cl.[F:2][C:3]1[CH:4]=[C:5]2[C:12](=[CH:13][CH:14]=1)[C:8]([CH2:9][CH2:10][NH2:11])=[CH:7][NH:6]2.O.[C:16](O)(=O)C=O.[OH-].[K+].Cl.[OH-].[Na+]>O>[F:2][C:3]1[CH:4]=[C:5]2[C:12]([C:8]3[CH2:9][CH2:10][NH:11][CH2:16][C:7]=3[NH:6]2)=[CH:13][CH:14]=1

참가 물질

7

반응물 5

HCID 313Hydrochloric Acid2회HCID 14797Potassium HydroxideHCID 14798Sodium HydroxideHCID 30850786-Fluoro-1H-indole-3-ethylamine monohydrochlorideHCID 15620607Glyoxylic acid, monohydrate

생성물 1

HCID 150775507-Fluoro-2,3,4,9-tetrahydro-1H-beta-carboline

시약·촉매·용매 1

HCID 962Water용매

실험 절차

6-Fluorotryptamine hydrochloride (0.511 g, 2.38 mmol) was dissolved in water (9 ml). Glyoxylic acid monohydrate (0.241 g, 2.618 mmol) was added, followed by KOH (0.129 g, 2.31 mmol). The resultant solid was stirred at ambient temperature for one hour before concentrated HCl (0.6 ml) was added in one portion. The mixture was refluxed for 30 minutes, more concentrated hydrogen chloride (0.6 ml) was added and the mixture was again refluxed for 15 minutes. The mixture was cooled to room temperature and basified to pH12 using 5N sodium hydroxide. It was extracted with chloroform (4×75 ml), separated, dried over magnesium sulphate, filtered and concentrated in vacuo to yield an off-white solid.

후처리

  1. additionwas added in one portion
  2. temperatureThe mixture was refluxed for 30 minutes
  3. temperaturethe mixture was again refluxed for 15 minutes
  4. extractionIt was extracted with chloroform (4×75 ml)
  5. customseparated
  6. dry with materialdried over magnesium sulphate
  7. filtrationfiltered
  8. concentrationconcentrated in vacuo
  9. customto yield an off-white solid

출처 및 근거

ORD 기록
ord-5662d6f74a0043c580236b8abd680190
출처 데이터셋
uspto-grants-1996_10
특허 번호
US05563147

연결된 노트

불러오는 중…