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Ethanol → Ethyl ester of lactic acid glycolic acid

HRID 234084
ノート
印刷プレビュー

反応式

HRID 234084 の反応式
[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]
参加物実験手順後処理出典と根拠反応ノート

参加物

7

反応物 3

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

生成物 1

HCID 131719795Ethyl ester of lactic acid glycolic acid収率 146.4%

試薬・触媒・溶媒 3

HCID 962Water溶媒HCID 6344Dichloromethane
溶媒
2 回
HCID 8471Triethylamine溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-38b6023ee63b4506908dd3ebfbe2100e
出典データセット
uspto-grants-1997_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05594091

反応ノート

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