Methanesulfonic Acid → 6,8-difluoro-N-methyl-2,3,4,9-tetrahydro-1H-carbazol-3-amine

HRID 128121

반응식

HRID 128121 반응식
[CH3:1][NH:2][CH:3]1[CH2:8][CH2:7][C:6](=O)[CH2:5][CH2:4]1.Cl.[F:11][C:12]1[CH:17]=[C:16]([F:18])[CH:15]=[CH:14][C:13]=1[NH:19]N.CS(O)(=O)=O>C(O)C>[CH3:1][NH:2][CH:3]1[CH2:8][C:7]2[C:14]3[C:13](=[C:12]([F:11])[CH:17]=[C:16]([F:18])[CH:15]=3)[NH:19][C:6]=2[CH2:5][CH2:4]1

참가 물질

5

반응물 3

HCID 6395Methanesulfonic AcidHCID 27333012,4-Difluorophenylhydrazine hydrochlorideHCID 207606324-(Methylamino)cyclohexanone

생성물 1

HCID 123618236,8-difluoro-N-methyl-2,3,4,9-tetrahydro-1H-carbazol-3-amine

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

A solution of 3.5 g. of 4-methylaminocyclohexanone, 5.1 g. of 2,4-difluorophenylhydrazine hydrochloride, and 4 g. of methanesulfonic acid in 50 ml. of absolute ethyl alcohol was heated under reflux for four hours, cooled, and filtered. The resulting solids were washed with isopropanol and treated in chloroform with 10% potassium hydroxide solution. The chloroform extract was evaporated to dryness to give 3-(methylamino)-6,8-difluoro-1,2,3,4-tetrahydrocarbazole, m.p. 135°-138° C., which was converted to the hydrochloride salt, m.p. >280° C.

후처리

  1. temperatureunder reflux for four hours
  2. temperaturecooled
  3. filtrationfiltered
  4. washThe resulting solids were washed with isopropanol
  5. additiontreated in chloroform with 10% potassium hydroxide solution
  6. extractionThe chloroform extract
  7. customwas evaporated to dryness

출처 및 근거

ORD 기록
ord-e4bf60a1cc6d4246af8dab5119fb820b
출처 데이터셋
uspto-grants-1981_03
특허 번호
US04257952

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