Hydrochloric Acid → 6-methoxy-2,3,4,5-tetrahydro-1H-3-benzazepine hydrochloride

HRID 1013095ノート

反応式

HRID 1013095 の反応式
[CH3:1][O:2][C:3]1[C:13]2[CH2:12][CH2:11][NH:10][CH2:9][CH2:8][C:7]=2[CH:6]=[CH:5][CH:4]=1.[ClH:14].CCCCCCC>C(O)C>[ClH:14].[CH3:1][O:2][C:3]1[C:13]2[CH2:12][CH2:11][NH:10][CH2:9][CH2:8][C:7]=2[CH:6]=[CH:5][CH:4]=1

参加物

5

反応物 3

HCID 313Hydrochloric AcidHCID 8900HeptaneHCID 138533586-Methoxy-2,3,4,5-tetrahydro-1H-3-benzazepine

生成物 1

HCID 574580206-methoxy-2,3,4,5-tetrahydro-1H-3-benzazepine hydrochloride収率 63%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒2 回

実験手順

Dissolve crude 6-methoxy-2,3,4,5-tetrahydro-1H-benzo[d]azepine (35.1 g, 0.198 mol) in ethanol (250 mL). Heat the solution to reflux and add 2 N HCl in ethanol (108.9 mL, 0.218 mol, 1.1 equiv.). Slowly add heptane (700 mL) over 10 min, then remove the heating mantle and cool the solution to RT and finally continue the cooling with an ice water mixture. Collect the resulting solid by vacuum filtration and wash with cold 1:2 ethanol:heptane (3×100 mL), dry for 15 min while applying vacuum suction, then further dry the product in a vacuum oven at 60° C. for 1 h to give the title compound as a white granular solid (35.53 g, 63%).

後処理

  1. temperatureHeat the solution
  2. temperatureto reflux
  3. customremove the heating mantle
  4. customCollect the resulting solid
  5. filtrationby vacuum filtration
  6. washwash with cold 1:2 ethanol
  7. dry with materialheptane (3×100 mL), dry for 15 min
  8. customfurther dry the product in a vacuum oven at 60° C. for 1 h

出典と根拠

ORDレコード
ord-42bd5e048db744538c1c8ac5a40e90de
出典データセット
uspto-grants-2011_07
特許番号
US07981882B2

反応ノート

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