Ethanol → Ethyl ester of lactic acid glycolic acid

HRID 234084

반응식

HRID 234084 반응식
[C:1]([OH:6])(=[O:5])[CH:2]([CH3:4])[OH:3].[C:7]([OH:11])(=[O:10])[CH2:8][OH:9].C(O)C.ClC(OCC)=O>O.ClCCl.C(N(CC)CC)C>[CH3:7][CH2:8][O:5][C:1]([CH:2]([OH:3])[CH3:4])=[O:6].[C:7]([OH:11])(=[O:10])[CH2:8][OH:9]

참가 물질

7

반응물 3

HCID 702EthanolHCID 10928Ethyl chloroformateHCID 36797Hydroxyacetic acid--2-hydroxypropanoic acid (1/1)2회

생성물 1

HCID 131719795Ethyl ester of lactic acid glycolic acid수율 146.4%

시약·촉매·용매 3

HCID 962Water용매HCID 6344Dichloromethane용매2회HCID 8471Triethylamine용매

실험 절차

9 g of a lactic acid/glycolic acid copolymer having a weight-average molecular weight of about 7,500 (lactic acid/glycolic acid=75/25 (mol %)) (Wako Pure Chemical Industries, Ltd.) was dissolved in a mixed solvent consisting of 20 ml of dichloromethane and 20 ml of ethanol. While thus obtained solution was cooled and stirred, 0.45 ml of triethyl amine, 0.29 ml of ethyl chloroformate and 0.36 g of N,N-dimethylaminopyridine were added. After the resulting mixture was stirred for another 2 hours, 50 ml of dichloromethane and 50 ml of water were added and then dichloromethane phase was separated. The dichloromethane phase was washed 2 times with 50 ml of 10% ethanol-water, and then dried with magnesium sulfate. After magnesium sulfate was separated by filtration, the mixture was concentrated to dryness under reduced pressure to yield 7.7 g of the ethyl ester of lactic acid/glycolic acid copolymer.

후처리

  1. dissolutionwas dissolved in a mixed solvent
  2. temperatureWhile thus obtained solution was cooled
  3. stirringAfter the resulting mixture was stirred for another 2 hours
  4. customdichloromethane phase was separated
  5. washThe dichloromethane phase was washed 2 times with 50 ml of 10% ethanol-water
  6. dry with materialdried with magnesium sulfate
  7. customAfter magnesium sulfate was separated by filtration
  8. concentrationthe mixture was concentrated to dryness under reduced pressure

출처 및 근거

ORD 기록
ord-38b6023ee63b4506908dd3ebfbe2100e
출처 데이터셋
uspto-grants-1997_01
특허 번호
US05594091

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