Benzaldehyde → Beta-Nitrostyrene

HRID 3305

反応式

HRID 3305 の反応式
[CH:1](=O)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[N+:9]([CH3:12])([O-:11])=[O:10].[OH-].[Na+].Cl>CO>[C:2]1([CH:1]=[CH:12][N+:9]([O-:11])=[O:10])[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1

参加物

6

反応物 4

HCID 240BenzaldehydeHCID 313Hydrochloric AcidHCID 6375NitromethaneHCID 14798Sodium Hydroxide

生成物 1

HCID 7626Beta-Nitrostyrene収率 37%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

反応条件

温度
-18 °C

実験手順

Benzaldehyde (10.0 g, 94.2 mmol) and nitromethane (5.1 mL, 94.2 mmol) were dissolved in MeOH, the solution was cooled to -18° C., and NaOH (3.9 g, 98.9 mmol) in aqueous solution (80 mL) was added while maintaining the temperature below -10° C. The mixture was stirred at 0° C. for 2 hours, then stored at 5° C. overnight. The solution was then poured into stirring acid (200 mL conc. HCl/300 mL H2O). The precipitate was collected, washed, and recrystallized from EtOH to afford the title compound as light orange needles (5.15 g, 37%).

後処理

  1. temperaturewhile maintaining the temperature below -10° C
  2. waitstored at 5° C. overnight
  3. additionThe solution was then poured
  4. customThe precipitate was collected
  5. washwashed
  6. customrecrystallized from EtOH

出典と根拠

ORDレコード
ord-e4c5a915e9a24293aae0af7d3e5b3bcb
出典データセット
uspto-grants-1998_03
特許番号
US05733912

関連ノート

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