Phosphorus oxychloride → Ethyl 2-chloro-4-methylquinoline-3-carboxylate

HRID 2304564노트

반응식

HRID 2304564 반응식
[CH3:1][C:2]1[C:11]2[C:6](=[CH:7][CH:8]=[CH:9][CH:10]=2)[NH:5][C:4](=O)[C:3]=1[C:13]([O:15][CH2:16][CH3:17])=[O:14].P(Cl)(Cl)([Cl:20])=O>>[Cl:20][C:4]1[C:3]([C:13]([O:15][CH2:16][CH3:17])=[O:14])=[C:2]([CH3:1])[C:11]2[C:6](=[CH:7][CH:8]=[CH:9][CH:10]=2)[N:5]=1

참가 물질

3

반응물 2

HCID 24813Phosphorus oxychlorideHCID 2794456HCID 2794456, 화합물

생성물 1

HCID 22987170Ethyl 2-chloro-4-methylquinoline-3-carboxylate

실험 절차

A suspension of ethyl 4-methyl-2-oxo-1,2-dihydro-3-quinolinecarboxylate (obtained according to 3.a, 15.2 g, 0.066 mol) in phosphoryl chloride (243 ml) is taken to reflux for 6 hours. The phosphoryl chloride is evaporated under reduced pressure without taking to dryness, and the viscous residue is poured into ice cold water (300 ml). The precipitate obtained in this way is filtered, washed with water to a neutral pH, then washed with ethanol and with diethyl ether in order to produce after drying 8.8 g (53%) of a white solid, m.p. 110° C.

후처리

  1. temperatureto reflux for 6 hours
  2. customThe phosphoryl chloride is evaporated under reduced pressure
  3. additionthe viscous residue is poured into ice cold water (300 ml)
  4. customThe precipitate obtained in this way
  5. filtrationis filtered
  6. washwashed with water to a neutral pH
  7. washwashed with ethanol and with diethyl ether in order
  8. customto produce
  9. dry with materialafter drying 8.8 g (53%) of a white solid, m.p. 110° C.

출처 및 근거

ORD 기록
ord-7d678373c2a042f69e9468d534f66af6
출처 데이터셋
uspto-grants-2002_08
특허 번호
US06436951B1

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