Acetone → 2-Methyl-5-vinylpyridine

HRID 325968Notes

Reaction equation

HRID 325968 reaction equation
[C:1](OC)(=O)C=C.C(O)(=O)C(C)=C.N[C@@H:14]([CH2:18][CH2:19][C:20]([NH:22][C@H:23]([C:26](NCC(O)=O)=O)[CH2:24]S)=O)C(O)=O.CC(C)=O>O.CO.CCCCCC>[CH3:26][C:23]1[CH:24]=[CH:1][C:19]([CH:18]=[CH2:14])=[CH:20][N:22]=1

Participants

8

Reactant 4

HCID 180AcetoneHCID 4093Methacrylic AcidHCID 7294Methyl AcrylateHCID 124886Glutathione

Product 1

HCID 88172-Methyl-5-vinylpyridine

Reagents, catalysts & solvents 3

HCID 887MethanolSolventHCID 962WaterSolvent2×HCID 8058HexaneSolvent

Procedure

methyl acrylate.methacrylic acid copolymer (molar ratio=2.4:1.9:1) (this copolymer being soluble in water at a pH lower than 4 or higher than 7 but not soluble in water at a pH of 4-7) and 100 g of ethylcellulose (ethoxy content: 48-50 w/w %) were dissolved in 2 liters of methanol, and 300 g of the glutathion-containing granules were dispersed therein. 2 liters of acetone and 8 liters of n-hexane were added gradually to the dispersion. The microcapsules thus formed were recovered by filtration, and washed with acetone-n-hexane (1:2) and n-hexane, successively. After said microcapsules were dried, microcapsules which passed through JIS standard sieve (500μ aperture) but did not pass through JIS standard sieve (105μ aperture) were collected. 467 g of glutathion-containing microcapsules which met the requirements of "Fine Granules" specified in THE PHARMACOPOEIA OF JAPAN 9th-Edition were thereby obtained.

Workup

  1. additionwere dispersed
  2. customThe microcapsules thus formed
  3. filtrationwere recovered by filtration
  4. washwashed with acetone-n-hexane (1:2) and n-hexane
  5. customwere dried
  6. customwere collected
  7. addition467 g of glutathion-containing microcapsules which
  8. customwere thereby obtained

Sources & evidence

ORD record
ord-225677b2b3614d9388f19aeaf162a2d3
Source dataset
uspto-grants-1984_04
Patent number
US04443497

Reaction notes

Loading…