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

HRID 128121

反応式

HRID 128121 の反応式
[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

参加物

5

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-e4bf60a1cc6d4246af8dab5119fb820b
出典データセット
uspto-grants-1981_03
特許番号
US04257952

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