Ammonia → 8-Nitro-2,3,4,5-tetrahydro-1H-1-benzazepine

HRID 423885

反応式

HRID 423885 の反応式
[NH:1]1[CH2:7][CH2:6][CH2:5][CH2:4][C:3]2[CH:8]=[CH:9][CH:10]=[CH:11][C:2]1=2.[N+:12]([O-])([O-:14])=[O:13].[K+].N>OS(O)(=O)=O>[N+:12]([C:10]1[CH:9]=[CH:8][C:3]2[CH2:4][CH2:5][CH2:6][CH2:7][NH:1][C:2]=2[CH:11]=1)([O-:14])=[O:13]

参加物

5

反応物 3

HCID 222AmmoniaHCID 24434Potassium NitrateHCID 5765032,3,4,5-tetrahydro-1H-1-benzazepine

生成物 1

HCID 468640718-Nitro-2,3,4,5-tetrahydro-1H-1-benzazepine収率 52%

試薬・触媒・溶媒 1

HCID 1118Sulfuric Acid溶媒

実験手順

At −10° C., 2,3,4,5-tetrahydro-1H-benzo[b]azepine (1.9 g, 13 mmol) was added dropwise to a solution of KNO3 (3 g, 30 mmol) in H2SO4 (50 mL). The mixture was stirred for 40 min, poured over crushed ice, basified with aq. ammonia to pH 13, and extracted with EtOAc. The combined organic phases were washed with brine, dried over Na2SO4 and concentrated to give 8-nitro-2,3,4,5-tetrahydro-1H-benzo[b]azepine as a black solid (1.3 g, 51%), which was used without further purification.

後処理

  1. additionpoured
  2. customover crushed ice
  3. extractionextracted with EtOAc
  4. washThe combined organic phases were washed with brine
  5. dry with materialdried over Na2SO4
  6. concentrationconcentrated

出典と根拠

ORDレコード
ord-df8129f99fb94400af951e60a4e601ac
出典データセット
uspto-grants-2012_01
特許番号
US08101767B2

関連ノート

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