Iodoethane → AD 1308

HRID 1732296노트

반응식

HRID 1732296 반응식
[C:1]1([C:7]2[C:16]3[C:11](=[CH:12][CH:13]=[CH:14][CH:15]=3)[N:10]=[C:9]([N:17]3[CH2:22][CH2:21][NH:20][CH2:19][CH2:18]3)[CH:8]=2)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.[CH2:23](I)[CH3:24].C(=O)([O-])[O-].[Na+].[Na+]>C(C(C)=O)C>[CH2:23]([N:20]1[CH2:19][CH2:18][N:17]([C:9]2[CH:8]=[C:7]([C:1]3[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=3)[C:16]3[C:11](=[CH:12][CH:13]=[CH:14][CH:15]=3)[N:10]=2)[CH2:22][CH2:21]1)[CH3:24]

참가 물질

5

반응물 3

HCID 6340IodoethaneHCID 10340Sodium CarbonateHCID 1662802-(1-Piperazinyl)-4-phenylquinolone

생성물 1

HCID 175033AD 1308수율 85.1%

시약·촉매·용매 1

HCID 6569Methyl Ethyl Ketone용매

실험 절차

A stirred suspension of 3.0 g of 4-phenyl-2-(1-piperazinyl)quinoline, 1.9 g of ethyl iodide and 1.1 g of sodium carbonate in 30 ml of methyl ethyl ketone was heated under reflux for 12 hours. The reaction mixture was concentrated under reduced pressure. To the residue was added water and the resulting mixture was extracted with ethyl acetate. The dried extracts were concentrated to give an oily residue, which was chromatographed on silica gel (30 g) using chloroform as an eluent. There was obtained the title compound (2.8 g, 85%), m.p. 87°-88° C.

후처리

  1. temperaturewas heated
  2. temperatureunder reflux for 12 hours
  3. concentrationThe reaction mixture was concentrated under reduced pressure
  4. additionTo the residue was added water
  5. extractionthe resulting mixture was extracted with ethyl acetate
  6. concentrationThe dried extracts were concentrated
  7. customto give an oily residue, which
  8. customwas chromatographed on silica gel (30 g)

출처 및 근거

ORD 기록
ord-238cde9c62334cc5a44a82d10219ddb6
출처 데이터셋
uspto-grants-1980_12
특허 번호
US04237135

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