Toluene → Neopentyl alpha-cyanoacrylate

HRID 486177노트

반응식

HRID 486177 반응식
[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]

참가 물질

6

반응물 3

HCID 1140TolueneHCID 6404Neopentyl alcoholHCID 9740Cyanoacetic acid

생성물 1

HCID 22266550Neopentyl alpha-cyanoacrylate수율 94%

시약·촉매·용매 2

HCID 1118Sulfuric Acid촉매HCID 962Water용매

실험 절차

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%).

후처리

  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

출처 및 근거

ORD 기록
ord-f60548f332b04c4e95c794f5c522112b
출처 데이터셋
uspto-grants-1994_03
특허 번호
US05290838

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