Glycerol → DL-3-n-Butylphthalide

HRID 1025245Notes

Reaction equation

HRID 1025245 reaction equation
O[CH2:2][CH:3]([CH2:5]O)O.[CH2:7]([O:9][C:10]([C:12]1[CH:18]=[CH:17][C:15](O)=[CH:14][CH:13]=1)=[O:11])[CH3:8]>O>[CH2:8]([CH:7]1[C:18]2[C:12](=[CH:13][CH:14]=[CH:15][CH:17]=2)[C:10](=[O:11])[O:9]1)[CH2:2][CH2:3][CH3:5]

Participants

4

Reactant 2

HCID 753GlycerolHCID 8434Ethylparaben

Product 1

HCID 61361DL-3-n-Butylphthalide

Reagents, catalysts & solvents 1

HCID 962WaterSolvent2×

Conditions

Temperature
75 °C

Procedure

100 g of gelatin, 30 g of glycerin, 130 g of water and 200 mg of ethylparaben are used. An appropriate amount of water is added into gelatin, allowing it to absorb water and to swell. Glycerin, ethylparaben and residual water are placed into a tank and heated to a temperature of 70 to 80° C., and homogeneously mixed. Swollen gelatin is added with agitation, melted, incubated for 1 to 2 hrs, and kept rest for foams to float up. The floating foams are then scraped, and the remainder is filtered through a clean white cloth and kept warm for further use. The viscosity of the resulting gum liquid is generally 2.8 to 3.2 degree.

Workup

  1. customto absorb water
  2. additionhomogeneously mixed
  3. additionSwollen gelatin is added with agitation
  4. filtrationthe remainder is filtered through a clean white cloth
  5. temperaturekept warm for further use
  6. customis generally 2.8 to 3.2 degree

Sources & evidence

ORD record
ord-a8767e884c874ba4a306100c1ed061b6
Source dataset
uspto-grants-2014_05
Patent number
US08728518B2

Reaction notes

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