Toluene → Neopentyl alpha-cyanoacrylate

HRID 486177ノート

反応式

HRID 486177 の反応式
[C:1]([CH2:3][C:4]([OH:6])=[O:5])#[N:2].[CH2:7](O)[C:8]([CH3:11])([CH3:10])[CH3:9].[C:13]1(C)C=CC=CC=1>S(=O)(=O)(O)O.O>[C:1]([C:3](=[CH2:13])[C:4]([O:6][CH2:7][C:8]([CH3:11])([CH3:10])[CH3:9])=[O:5])#[N:2]

参加物

6

反応物 3

HCID 1140TolueneHCID 6404Neopentyl alcoholHCID 9740Cyanoacetic acid

生成物 1

HCID 22266550Neopentyl alpha-cyanoacrylate収率 94%

試薬・触媒・溶媒 2

HCID 1118Sulfuric Acid触媒HCID 962Water溶媒

実験手順

51 g (0.6 mole) of cyanoacetic acid, 74 g (0.84 mole) of neopentyl alcohol, 1 g of sulfuric acid and 100 g of toluene were reacted under reflux and water produced was removed by azeotropic distillation. Thereafter, the mixture thus produced was cooled to a room temperature and filtered to remove insoluble matter. The filtrate was washed with water and dried overnight with magensium sulfate. Then, the desiccant was filtered off and the solvent was removed under a reduced pressure, followed by vacuum distillation to afford 87.1 g of neopentyl α-cyanoacrylate (b.p. 79°-81° C./3 mmHg, yield 94%).

後処理

  1. temperatureunder reflux
  2. customwas removed by azeotropic distillation
  3. customThereafter, the mixture thus produced
  4. filtrationfiltered
  5. customto remove insoluble matter
  6. washThe filtrate was washed with water
  7. dry with materialdried overnight with magensium sulfate
  8. filtrationThen, the desiccant was filtered off
  9. customthe solvent was removed under a reduced pressure
  10. distillationfollowed by vacuum distillation

出典と根拠

ORDレコード
ord-f60548f332b04c4e95c794f5c522112b
出典データセット
uspto-grants-1994_03
特許番号
US05290838

反応ノート

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