Hydrochloric Acid → Methyl 7-bromo-2,3-dihydro-1H-1-benzazepine-4-carboxylate

HRID 586833ノート

反応式

HRID 586833 の反応式
[Br:1][C:2]1[CH:3]=[CH:4][C:5]2[N:11](C(OC(C)(C)C)=O)[CH2:10][CH2:9][C:8]([C:19]([O:21][CH3:22])=[O:20])=[CH:7][C:6]=2[CH:23]=1.Cl.[OH-].[Na+]>C(OCC)(=O)C>[Br:1][C:2]1[CH:3]=[CH:4][C:5]2[NH:11][CH2:10][CH2:9][C:8]([C:19]([O:21][CH3:22])=[O:20])=[CH:7][C:6]=2[CH:23]=1

参加物

5

反応物 3

HCID 313Hydrochloric AcidHCID 14798Sodium HydroxideHCID 22329270HCID 22329270、化合物

生成物 1

HCID 22328963Methyl 7-bromo-2,3-dihydro-1H-1-benzazepine-4-carboxylate収率 90.3%

試薬・触媒・溶媒 1

HCID 8857Ethyl Acetate溶媒

反応条件

温度
80 °C

実験手順

In ethyl acetate (50 ml) was dissolved methyl 7-bromo-1-(t-butoxycarbonyl)-2,3-dihydro-1H-1-benzazepine-4-carboxylate (1.5 g). To the solution was added 6N hydrochloric acid (2 ml), and the mixture was heated to stir at 80° C. for 2 hours, neutralized with 1N sodium hydroxide solution and extracted with ethyl acetate. The organic layer was washed with water and saturated brine and dried with anhydrous magnesium sulfate. The solvent was evaporated to give methyl 7-bromo-2,3-dihydro-1H-1-benzazepine-4-carboxylate (1.0 g) as yellow crystals.

後処理

  1. temperaturethe mixture was heated
  2. extractionextracted with ethyl acetate
  3. washThe organic layer was washed with water and saturated brine
  4. dry with materialdried with anhydrous magnesium sulfate
  5. customThe solvent was evaporated

出典と根拠

ORDレコード
ord-9d37eefaa9f248b6b2a0bcd0c35b94d2
出典データセット
uspto-grants-2005_08
特許番号
US06936602B1

反応ノート

読み込み中…