Hydroquinone → Acrylamidoglycolic acid Methyl Ether

HRID 868291노트

반응식

HRID 868291 반응식
[C:1]([NH:5][CH:6]([OH:10])[C:7]([OH:9])=[O:8])(=[O:4])[CH:2]=[CH2:3].[CH3:11]OC(OC)OC.COC.C1(C=CC(O)=CC=1)O>CO>[CH3:11][O:10][CH:6]([NH:5][C:1](=[O:4])[CH:2]=[CH2:3])[C:7]([OH:9])=[O:8]

참가 물질

6

반응물 4

HCID 785HydroquinoneHCID 8254Dimethyl EtherHCID 9005Trimethyl orthoformateHCID 92230Acetic acid, 2-hydroxy-2-[(1-oxo-2-propen-1-yl)amino]-

생성물 1

HCID 19933811Acrylamidoglycolic acid Methyl Ether

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

45 parts of acrylamidoglycolic acid, 90 parts trimethylorthoformate, 0.045 parts of the mono methyl ether of hydroquinone and 35 parts of methanol are mixed in a flask equipped with a stirrer, condensor and thermometer. The mixture was heated at a bath temperature of 60°-65° C. for 24 hours. A small amount of insoluble material was filtered off and discarded. The filtrate was stripped of solvent under vacuum and a rubbery substance was obtained. This material was extracted with ether with stirring for 3 days. The solid which was insoluble in the ether was filtered off and was further extracted with acetone. The acetone was removed to yield 24 g of crude AGME (Mp. 100-102.5).

후처리

  1. customequipped with a stirrer
  2. temperatureThe mixture was heated at a bath temperature of 60°-65° C. for 24 hours
  3. filtrationA small amount of insoluble material was filtered off
  4. customa rubbery substance was obtained
  5. extractionThis material was extracted with ether
  6. filtrationwas filtered off
  7. extractionwas further extracted with acetone
  8. customThe acetone was removed
  9. customto yield 24 g of crude AGME (Mp. 100-102.5)

출처 및 근거

ORD 기록
ord-3ab54f0a536c4abaac2c3886d17842a7
출처 데이터셋
uspto-grants-1988_10
특허 번호
US04778869

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