Methylamine → HCID 21493546, 화합물

HRID 1973255노트

반응식

HRID 1973255 반응식
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

참가 물질

4

반응물 2

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

생성물 1

HCID 21493546HCID 21493546, 화합물

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

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°.

후처리

  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

출처 및 근거

ORD 기록
ord-261de9e471a142768f627eaf94d41fa4
출처 데이터셋
uspto-grants-1976_12
특허 번호
US03996373

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