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Potassium Carbonate → Hexahydro-1-(3-methyl-4-nitrophenyl)-1H-1,4-diazepine

HRID 1294399
ノート
印刷プレビュー

反応式

HRID 1294399 の反応式
F[C:2]1[CH:7]=C[CH:5]=[CH:4][C:3]=1[N+:8]([O-:10])=[O:9].C(=O)([O-])[O-].[K+].[K+].[C:17]([N:20]1[CH2:26][CH2:25][CH2:24][NH:23][CH2:22][CH2:21]1)(=O)[CH3:18]>O>[CH3:5][C:4]1[CH:18]=[C:17]([N:20]2[CH2:26][CH2:25][CH2:24][NH:23][CH2:22][CH2:21]2)[CH:7]=[CH:2][C:3]=1[N+:8]([O-:10])=[O:9]
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 11430Potassium CarbonateHCID 738951-Fluoro-2-nitrobenzeneHCID 4186202N-Acetylhomopiperazine

生成物 1

HCID 13007953Hexahydro-1-(3-methyl-4-nitrophenyl)-1H-1,4-diazepine収率 53.6%

試薬・触媒・溶媒 1

HCID 962Water溶媒

反応条件

温度
95 °C

実験手順

Fluoronitrobenzene (9.1 g, 0.0586 mol) is dissolved in water (50 ml) and then potassium carbonate (9.7 9, 0.0703 mol) and 1-acetyl-[1,4]diazepane (10 g, 0.0703 mol) are added. The medium is heated at 95° C. for 6 hours, and an orange-coloured solution is obtained. The medium is then cooled to room temperature, and an orange-coloured sticky paste then appears. The maximum amount of water is removed from the reaction medium. Isopropanol is then added to the paste until a yellow solid precipitates. The medium is filtered and, after drying in a vacuum oven at 45° C., a yellow powder is obtained which corresponds to 1-(3-methyl-4-nitrophenyl)-[1,4]diazepane (1). (8.7 g; Yield=53.6%)

後処理

  1. customan orange-coloured solution is obtained
  2. temperatureThe medium is then cooled to room temperature
  3. customThe maximum amount of water is removed from the reaction medium
  4. additionIsopropanol is then added to the paste until a yellow solid
  5. customprecipitates
  6. filtrationThe medium is filtered
  7. customafter drying in a vacuum oven at 45° C.

出典と根拠

ORDレコード
ord-4e180161d1a043528d320aa611ce7a1a
出典データセット
uspto-grants-2007_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07241317B2

反応ノート

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