Malonic Acid → HCID 20517749, 화합물

HRID 2198878노트

반응식

HRID 2198878 반응식
[C:1]([OH:4])(=[O:3])[CH3:2].O[C:6]1[CH:19]=[C:18]2[C:9]([CH:10]=[CH:11][C:12]3[O:13][CH:14]=[C:15](C=O)[C:16](=[O:20])[C:17]=32)=[CH:8][CH:7]=1.[C:23](O)(=O)[CH2:24][C:25]([OH:27])=[O:26]>N1C=CC=CC=1>[C:1]([O:4][C:6]1[CH:19]=[C:18]2[C:9]([CH:10]=[CH:11][C:12]3[O:13][CH:14]=[C:15]([C:24](=[CH2:23])[C:25]([OH:27])=[O:26])[C:16](=[O:20])[C:17]=32)=[CH:8][CH:7]=1)(=[O:3])[CH3:2]

참가 물질

4

반응물 2

HCID 867Malonic Acid2회HCID 867372399-hydroxy-1-oxo-1H-naphtho[2,1-b]pyran-2-carboxaldehyde acetate

생성물 1

HCID 20517749HCID 20517749, 화합물수율 25.5%

시약·촉매·용매 1

HCID 1049Pyridine용매

실험 절차

A mixture of 9-hydroxy-1-oxo-1H-naphtho[2,1-b]pyran-2-carboxaldehyde acetate (10.0 g, 0.0354 m) and malonic acid (4.0 g, 0.0354 m) in pyridine (100 ml) is refluxed for 45 minutes. Additional malonic acid (1.0 g, 0.00885 m, 0.25 eq.) is added and the reaction refluxed for 30 minutes. The solvent is removed under reduced pressure to give a sludge from which product crystallizes on the addition of acetone. After filtering the product, recrystallization from DMF gives cocoa crystals (2.75 g, 24%), m.p. dec>290° C.

후처리

  1. temperatureis refluxed for 45 minutes
  2. temperaturethe reaction refluxed for 30 minutes
  3. customThe solvent is removed under reduced pressure
  4. customto give a sludge from which product
  5. customcrystallizes on the addition of acetone
  6. filtrationAfter filtering
  7. customthe product, recrystallization from DMF

출처 및 근거

ORD 기록
ord-e4e8062f30fa48399586d60bb6ab6171
출처 데이터셋
uspto-grants-1982_11
특허 번호
US04360527

반응 노트

불러오는 중…