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

HRID 220784ノート

反応式

HRID 220784 の反応式
[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

参加物

4

反応物 2

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

(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%).

後処理

  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

出典と根拠

ORDレコード
ord-8d1cb204aea94ec686d6fbc7019208dc
出典データセット
uspto-grants-2012_06
特許番号
US08202858B2

反応ノート

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