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llms.txt · MCP 가이드개인정보처리방침 · 이용약관 · 지원v1.8.0
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5-ethyl-5-hydroxy-9-methoxy-4,5-dihydrooxepino[3,4-c]pyridin-3(1H)-one → 5-Ethyl-5-hydroxy-1,4,5,8-tetrahydrooxepino[3,4-c]pyridine-3,9-dione

HRID 720495
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인쇄 미리보기

반응식

HRID 720495 반응식
[CH2:1]([C:3]1([OH:17])[C:13]2[C:8](=[C:9]([O:14]C)[N:10]=[CH:11][CH:12]=2)[CH2:7][O:6][C:5](=[O:16])[CH2:4]1)[CH3:2]>Cl>[CH2:1]([C:3]1([OH:17])[C:13]2[CH:12]=[CH:11][NH:10][C:9](=[O:14])[C:8]=2[CH2:7][O:6][C:5](=[O:16])[CH2:4]1)[CH3:2]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

3

반응물 1

HCID 105618445-ethyl-5-hydroxy-9-methoxy-4,5-dihydrooxepino[3,4-c]pyridin-3(1H)-one

생성물 1

HCID 105370475-Ethyl-5-hydroxy-1,4,5,8-tetrahydrooxepino[3,4-c]pyridine-3,9-dione수율 49.1%

시약·촉매·용매 1

HCID 313Hydrochloric Acid용매

실험 절차

5-Ethyl-5-hydroxy-9-methoxy-4,5-dihydrooxepino[3,4-c]pyridin-3(1H)-one (0.5 g, 2.1 mmol) is heated under reflux for 9 hours in 1N hydrochloric acid (20 ml). The reaction mixture is concentrated under reduced pressure and the residue is again dried by the addition and evaporation of toluene twice, then left overnight under reduced pressure in the presence of phosphorus pentoxide. The resultant oil is dissolved in anhydrous acetonitrile (5 ml) and agitated under argon for 24 hours. The precipitate is filtered out and dried, which produces 0.23 g (49%) of a white solid (M), m.p. 118–119° C.

후처리

  1. concentrationThe reaction mixture is concentrated under reduced pressure
  2. dry with materialthe residue is again dried by the addition and evaporation of toluene twice
  3. dissolutionThe resultant oil is dissolved in anhydrous acetonitrile (5 ml)
  4. filtrationThe precipitate is filtered out
  5. customdried

출처 및 근거

ORD 기록
ord-824e69e4bf1748f9bcd68f27380683a9
출처 데이터셋
uspto-grants-2006_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07135478B2

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