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Methanol → HCID 11287403, 화합물

HRID 1265399
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인쇄 미리보기

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HRID 1265399 반응식
[C:1]([O:6][CH3:7])(=[O:5])[CH:2]([CH3:4])[OH:3].[C:8]1(=[O:14])[O:13][C:11](=[O:12])[CH2:10][CH2:9]1.CO.[C:17]([O-])([O-])=O.[Ca+2]>S(=O)(=O)(O)O.C(Cl)(Cl)Cl>[CH3:17][O:13][C:11](=[O:12])[CH2:10][CH2:9][C:8]([O:3][CH:2]([C:1]([O:6][CH3:7])=[O:5])[CH3:4])=[O:14]
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 4

HCID 887MethanolHCID 7922Succinic anhydrideHCID 10112Calcium CarbonateHCID 11040Methyl Lactate

생성물 1

HCID 11287403HCID 11287403, 화합물

시약·촉매·용매 2

HCID 1118Sulfuric Acid촉매HCID 6212
Chloroform
용매

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온도
70 °C

실험 절차

Methyl lactate (14 mL, 0.147 moles), succinic anhydride (14.76 g, 0.147 moles), and 2 drops of concentrated sulfuric acid were mixed and heated to 70° C. for five hours. An NMR spectrum of a sample of the cooled reaction mixture showed quantitative conversion to succinic acid (ethyl-1-methoxycarbonyl) ester. Methanol (30 mL) and chloroform (20 mL) were added and heated to reflux in a soxhlet extractor containing silica gel in the receiver. The solution was refluxed for three hours, neutralized with CaCO3, filtered, and the volatile solvents removed under vacuum. The isolated yield of (i) was 29.56 g (98.5%).

후처리

  1. customAn NMR spectrum of a sample of the cooled reaction mixture
  2. temperatureheated
  3. temperatureto reflux in a soxhlet extractor
  4. additioncontaining silica gel in the receiver
  5. temperatureThe solution was refluxed for three hours
  6. filtrationfiltered
  7. customthe volatile solvents removed under vacuum

출처 및 근거

ORD 기록
ord-7406d3e57b87463e9954cf6936325c90
출처 데이터셋
uspto-grants-2003_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06545175B1

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