Potassium Carbonate → 7-Methoxy-2,3,4,5-tetrahydro-1H-2-benzazepin-1-one

HRID 6764

反応式

HRID 6764 の反応式
[N-:1]=[N+]=[N-].[Na+].[CH3:5][O:6][C:7]1[CH:8]=[C:9]2[C:14](=[CH:15][CH:16]=1)[C:13](=[O:17])[CH2:12][CH2:11][CH2:10]2.C(=O)([O-])[O-].[K+].[K+]>Cl>[CH3:5][O:6][C:7]1[CH:16]=[CH:15][C:14]2[C:13](=[O:17])[NH:1][CH2:12][CH2:11][CH2:10][C:9]=2[CH:8]=1

参加物

5

反応物 3

HCID 11430Potassium CarbonateHCID 141126-Methoxy-alpha-tetraloneHCID 33557Sodium Azide

生成物 1

HCID 42306097-Methoxy-2,3,4,5-tetrahydro-1H-2-benzazepin-1-one

試薬・触媒・溶媒 1

HCID 313Hydrochloric Acid溶媒

実験手順

Sodium azide (0.37 g) was slowly added in portions to a stirring ice-cold suspension of 6-methoxy-3,4-dihydro-2H-naphthalen-1-one in 10 mL of concentrated hydrochloric acid. The mixture was allowed to slowly warm to room temperature and stirred for 20 h. The mixture was poured onto ice and carefully neutralized with solid potassium carbonate. The resulting mixture was extracted with two 50 mL aliquots of dichloromethane. The organic material was dried over sodium sulfate and the solvent was evaporated. Chromatography (ethyl acetate) gave 0.45 g of 7-methoxy-2,3,4,5-tetrahydrobenzo[c]azepine-1-one.

後処理

  1. additionThe mixture was poured onto ice
  2. extractionThe resulting mixture was extracted with two 50 mL aliquots of dichloromethane
  3. dry with materialThe organic material was dried over sodium sulfate
  4. customthe solvent was evaporated

出典と根拠

ORDレコード
ord-141213c897394fb3aee98326e828dc45
出典データセット
uspto-grants-2006_08
特許番号
US07084154B2

関連ノート

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