Methylamine → HCID 21493546、化合物

HRID 1973255ノート

反応式

HRID 1973255 の反応式
Br[CH2:2][C:3]1[C:4]2[C:9]([C:10]3[CH:11]=[CH:12][CH:13]=[CH:14][C:15]=3[C:16]=1[CH2:17]Br)=[CH:8][CH:7]=[CH:6][CH:5]=2.[CH3:19][NH2:20]>CO>[CH3:19][N:20]1[CH2:17][C:16]2[C:3](=[C:4]3[CH:5]=[CH:6][CH:7]=[CH:8][C:9]3=[C:10]3[CH:11]=[CH:12][CH:13]=[CH:14][C:15]3=2)[CH2:2]1

参加物

4

反応物 2

HCID 6329MethylamineHCID 4663482Phenanthrene, 9,10-bis(bromomethyl)-

生成物 1

HCID 21493546HCID 21493546、化合物

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

13.4 g of 9,10-bis-bromomethyl-phenanthrene [see S. Hauptmann, Chem. Ber. 93, 2604 (1960)] is added within one hour, with stirring, to a solution of 37.5 g of methylamine in 225 ml of methanol, with the reaction temperature being maintained at 45°-50°. The reaction mixture is stirred for a further hour at 50°, and the solvent and excess methylamine are subsequently distilled off. 50 ml of water is added to the residue, and the formed suspension is extracted with ether. The ethereal solution is washed with water, dried over potassium carbonate and concentrated by evaporation. The residue is recrystallised from acetone to yield 2-methyl-2,3-dihydro-1H-dibenz[e,g]isoindole, m.p. 122°-123°.

後処理

  1. temperaturebeing maintained at 45°-50°
  2. distillationthe solvent and excess methylamine are subsequently distilled off
  3. addition50 ml of water is added to the residue
  4. extractionthe formed suspension is extracted with ether
  5. washThe ethereal solution is washed with water
  6. dry with materialdried over potassium carbonate
  7. concentrationconcentrated by evaporation
  8. customThe residue is recrystallised from acetone

出典と根拠

ORDレコード
ord-261de9e471a142768f627eaf94d41fa4
出典データセット
uspto-grants-1976_12
特許番号
US03996373

反応ノート

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