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llms.txt · MCP 가이드개인정보처리방침 · 이용약관 · 지원v1.8.0
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Acetic Acid → Y 9000

HRID 1579390
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반응식

HRID 1579390 반응식
C(O)(=O)C.S(=O)(=O)(O)O.[O:10]=[C:11]1[C:20]2[C:15](=[N:16][CH:17]=[CH:18][CH:19]=2)[O:14][C:13]2[CH:21]=[CH:22][C:23]([C:25]([CH:27](C(OCC)=O)C(OCC)=O)=[O:26])=[CH:24][C:12]1=2>O>[C:25]([C:23]1[CH:22]=[CH:21][C:13]2[O:14][C:15]3=[N:16][CH:17]=[CH:18][CH:19]=[C:20]3[C:11](=[O:10])[C:12]=2[CH:24]=1)(=[O:26])[CH3:27]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 176Acetic AcidHCID 1118Sulfuric AcidHCID 21568404HCID 21568404, 화합물

생성물 1

HCID 198324Y 9000

시약·촉매·용매 1

HCID 962Water용매2회

실험 절차

A mixture of 7.5 ml of glacial acetic acid, 0.9 ml of concentrated sulfuric acid, 4.5 ml of water and 4.6 g of diethyl 2-(5-oxo-5H-[1]benzopyrano[2,3-b]pyridin-7-yl-carbonyl)malonate is stirred under reflux for 2 hours. The reaction mixture is poured into 50 ml of cool water. The crystalline precipitate is filtered off, and suspended in water. The suspension is alkalified with 10% sodium hydroxide under ice cooling, and extracted with chloroform. The extract is washed thoroughly with water, dried, and concentrated. The residue is recrystallized from toluene to give 7 -acetyl-5-oxo-5H-[1]benzopyrano[2,3-b]pyridine melting at 194°-195°C.

후처리

  1. temperatureunder reflux for 2 hours
  2. filtrationThe crystalline precipitate is filtered off
  3. extractionextracted with chloroform
  4. washThe extract is washed thoroughly with water
  5. customdried
  6. concentrationconcentrated
  7. customThe residue is recrystallized from toluene

출처 및 근거

ORD 기록
ord-adba64faaa814d8fb4314aba66ca6464
출처 데이터셋
uspto-grants-1976_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US03931199

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