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Hydrochloric Acid → 7-Bromo-1-formyl-2,3-dihydro-1-benzazepine-4-carboxylic acid

HRID 1277318
ノート
印刷プレビュー

反応式

HRID 1277318 の反応式
[Br:1][C:2]1[CH:3]=[CH:4][C:5]2[N:11]([CH:12]=[O:13])[CH2:10][CH2:9][C:8]([C:14]([O:16]CC)=[O:15])=[CH:7][C:6]=2[CH:19]=1.Cl>[OH-].[Na+].C1COCC1.C(O)C>[Br:1][C:2]1[CH:3]=[CH:4][C:5]2[N:11]([CH:12]=[O:13])[CH2:10][CH2:9][C:8]([C:14]([OH:16])=[O:15])=[CH:7][C:6]=2[CH:19]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 2

HCID 313Hydrochloric AcidHCID 18472216Ethyl 7-bromo-1-formyl-2,3-dihydro-1-benzazepine-4-carboxylate

生成物 1

HCID 184725177-Bromo-1-formyl-2,3-dihydro-1-benzazepine-4-carboxylic acid収率 100%

試薬・触媒・溶媒 2

HCID 14798Sodium Hydroxide溶媒HCID 21873804Tetrahydrofuran ethanol溶媒

実験手順

In 1N sodium hydroxide (13.0 ml) and THF:ethanol (1:1, 50 ml) was dissolved ethyl 7-bromo-1-formyl-2,3-dihydro-1-benzazepine-4-carboxylate (2.77 g), and the mixture was stirred at room temperature for 15 hours. To the mixture was added 1N hydrochloric acid (12.5 ml), and the mixture was concentrated. To the residue was added water (200 ml), and the mixture was adjusted to pH 2 with 1N hydrochloric acid. The mixture was extracted with ethyl acetate(300 ml×3), and the organic layer was dried with magnesium sulfate. The solvent was evaporated under reduced pressure to give 7-bromo-1-formyl-2,3-dihydro-1-benzazepine-4-carboxylic acid (2.52 g, 100%).

後処理

  1. concentrationthe mixture was concentrated
  2. additionTo the residue was added water (200 ml)
  3. extractionThe mixture was extracted with ethyl acetate(300 ml×3)
  4. dry with materialthe organic layer was dried with magnesium sulfate
  5. customThe solvent was evaporated under reduced pressure

出典と根拠

ORDレコード
ord-d90ee5bca5774e78a6ac760e90fc5430
出典データセット
uspto-grants-2000_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06166006

反応ノート

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