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Methanol → Methyl acrylamidoglycolate methyl ether

HRID 868288
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HRID 868288 반응식
[C:1]([NH:5][CH:6](O)[C:7]([OH:9])=[O:8])(=[O:4])[CH:2]=[CH2:3].[CH:11]1C2NC3C(=CC=CC=3)SC=2C=CC=1.S(=O)(=O)(O)O.C(=O)([O-])[O-].[Na+].[Na+].[CH3:36][OH:37]>C(Cl)(Cl)Cl>[CH3:36][O:37][CH:6]([NH:5][C:1](=[O:4])[CH:2]=[CH2:3])[C:7]([O:9][CH3:11])=[O:8]
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 5

HCID 887MethanolHCID 1118Sulfuric AcidHCID 7108PhenothiazineHCID 10340Sodium CarbonateHCID 92230Acetic acid, 2-hydroxy-2-[(1-oxo-2-propen-1-yl)amino]-

생성물 1

HCID 156893Methyl acrylamidoglycolate methyl ether

시약·촉매·용매 1

HCID 6212
Chloroform
용매

반응 조건

온도
40 °C

실험 절차

To a three-necked flask equipped with a stirrer and an extractor filled with a molecular sieve drying agent was added 300 parts acrylamidoglycolic acid, 3000 parts methanol, 0.05 parts phenothiazine, 4.5 parts 98% sulfuric acid and 200 parts chloroform. The mixture was heated to reflux and the distillate was allowed to pass through the extractor for 61/2 hours. The mixture was cooled and allowed to stand for 16 hours at which point the mixture was warmed to about 40° C., 19 g of sodium carbonate was added, and the solution was stirred for 21/2 hours. The mixture was filtered and vacuum stripped of solvent. The solid residue was extracted with chloroform. Diethyl ether was added to the extract and a polymeric mass precipitated which was discarded. The remaining extract was stripped of solvent to yield 264.2 parts of crude MAGME which was confirmed by chemical analysis.

후처리

  1. customTo a three-necked flask equipped with a stirrer
  2. additionan extractor filled with a molecular sieve drying agent
  3. temperatureThe mixture was heated
  4. temperatureto reflux
  5. custom2 hours
  6. temperatureThe mixture was cooled
  7. filtrationThe mixture was filtered
  8. extractionThe solid residue was extracted with chloroform
  9. additionDiethyl ether was added to the
  10. extractionextract
  11. customa polymeric mass precipitated which
  12. extractionThe remaining extract

출처 및 근거

ORD 기록
ord-1918a24484e44c0ebda837638b739fe7
출처 데이터셋
uspto-grants-1988_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04778869

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