Silicon carbide → 2,4,5-Trimethoxyaniline

HRID 986633

反応式

HRID 986633 の反応式
[CH3:1][O:2][C:3]1[CH:8]=[C:7]([O:9][CH3:10])[C:6]([O:11][CH3:12])=[CH:5][C:4]=1[N+:13]([O-])=O.[C-]#[Si+].[OH-].[Na+]>Cl>[CH3:1][O:2][C:3]1[CH:8]=[C:7]([O:9][CH3:10])[C:6]([O:11][CH3:12])=[CH:5][C:4]=1[NH2:13]

参加物

5

反応物 3

HCID 9863Silicon carbideHCID 14798Sodium HydroxideHCID 8224151,2,4-Trimethoxy-5-nitrobenzene

生成物 1

HCID 124101382,4,5-Trimethoxyaniline

試薬・触媒・溶媒 1

HCID 313Hydrochloric Acid溶媒

実験手順

Into a 500 cm3 flask, provided with a cooling device, were added successively 21.3 g (0.1 mole) of 2,4,5-trimethoxy nitrobenzene, 80 g of chemically pure stannous chloride for mirror making, 100 cm3 of a hydrochloric acid solution (d=1.18) and carborundum. The mixture was brought to boiling under reflux for 1 h. After cooling, a caustic soda solution was added until the precipitate disolved. The solution obtained was extracted with methylene chloride. The organic extracts were dried over sodium sulfate then evaporated under reduced pressure. The residue obtained was crystallized in ethanol.

後処理

  1. customInto a 500 cm3 flask, provided with a cooling device
  2. temperatureunder reflux for 1 h
  3. temperatureAfter cooling
  4. customThe solution obtained
  5. extractionwas extracted with methylene chloride
  6. dry with materialThe organic extracts were dried over sodium sulfate
  7. customthen evaporated under reduced pressure
  8. customThe residue obtained
  9. customwas crystallized in ethanol

出典と根拠

ORDレコード
ord-4a9620286f364daf8a781c1aa480f17a
出典データセット
uspto-grants-1987_12
特許番号
US04714700

関連ノート

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