Hydrochloric Acid → 1-Benzyl-2-methyl-1,4,5,6-tetrahydro-1,3,6-triaza-benzo[e]azulene

HRID 220784노트

반응식

HRID 220784 반응식
[CH2:1]([N:8]1[C:17]2[C:16]3[CH:18]=[CH:19][CH:20]=[CH:21][C:15]=3[N:14](C(C3C=CC=CC=3)=O)[CH2:13][CH2:12][C:11]=2[N:10]=[C:9]1[CH3:30])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.Cl>CO>[CH2:1]([N:8]1[C:17]2[C:16]3[CH:18]=[CH:19][CH:20]=[CH:21][C:15]=3[NH:14][CH2:13][CH2:12][C:11]=2[N:10]=[C:9]1[CH3:30])[C:2]1[CH:3]=[CH:4][CH:5]=[CH:6][CH:7]=1

참가 물질

4

반응물 2

HCID 313Hydrochloric AcidHCID 57555380(1-Benzyl-2-methyl-4,5-dihydro-1H-1,3,6-triaza-benzo[e]azulen-6-yl)-phenyl-methanone

생성물 1

HCID 575554001-Benzyl-2-methyl-1,4,5,6-tetrahydro-1,3,6-triaza-benzo[e]azulene수율 78%

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

(1-Benzyl-2-methyl-4,5-dihydro-1H-1,3,6-triaza-benzo[e]azulen-6-yl)-phenyl-methanone from Example E5a.1 (5.73 g, 14.6 mmol) was placed in methanol (50 ml) and a 6M HCl aqueous solution (200 ml) was added. The reaction mixture was heated at reflux for 18 h then concentrated in vacuo. The residue was dissolved in dichloromethane, basified with saturated NaHCO3 then washed with brine, dried and concentrated in vacuo to yield the title compound (3.30 g, 78%).

후처리

  1. temperatureThe reaction mixture was heated
  2. temperatureat reflux for 18 h
  3. concentrationthen concentrated in vacuo
  4. dissolutionThe residue was dissolved in dichloromethane
  5. washthen washed with brine
  6. customdried
  7. concentrationconcentrated in vacuo

출처 및 근거

ORD 기록
ord-8d1cb204aea94ec686d6fbc7019208dc
출처 데이터셋
uspto-grants-2012_06
특허 번호
US08202858B2

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