1,8-Diazabicyclo(5.4.0)undec-7-ene → HCID 13071762, 화합물

HRID 2418470노트

반응식

HRID 2418470 반응식
[CH2:1]([O:3][C:4]([C:6]1[C:15](=[O:16])[C:14]2[C:9](=[CH:10][C:11]([Cl:18])=[C:12]([F:17])[CH:13]=2)[N:8]([CH2:19][CH2:20]Cl)[CH:7]=1)=[O:5])[CH3:2].C1CCN2C(=NCCC2)CC1>CS(C)=O>[CH2:1]([O:3][C:4]([C:6]1[C:15](=[O:16])[C:14]2[C:9](=[CH:10][C:11]([Cl:18])=[C:12]([F:17])[CH:13]=2)[N:8]([CH:19]=[CH2:20])[CH:7]=1)=[O:5])[CH3:2]

참가 물질

4

반응물 2

HCID 811841,8-Diazabicyclo(5.4.0)undec-7-eneHCID 6212337-Chloro-1-(2-chloroethyl)-6-fluoro-4-oxo-1,4-dihydroquinoline-3-carboxylic acid, ethyl ester

생성물 1

HCID 13071762HCID 13071762, 화합물수율 65.1%

시약·촉매·용매 1

HCID 679Dimethyl Sulfoxide용매

실험 절차

To a 120 ml of anhydrous dimethyl sulfoxide (DMSO), 6.32 g of 1-(2-chloroethyl)-6-fluoro-7-chloro-4-oxo-1,4-dihydroquinoline-3-carboxylic acid ethyl ester and 2.89 g of 1,8-diazabicyclo[5,4,0]-7-undecene were added and the mixture was heated at 84°-89° C. for 2 hrs. The reaction mixture was concentrated in vacuo and the residue was dissolved in chloroform. The chloroform layer was washed with water and dried. The residue obtained through evaporation of chloroform was recrystallized from ethyl ether to give 3.66 g (65.1% yield) of 1-vinyl-6-fluoro-7-chloro-4-oxo-1,4-dihydroquinoline-3-carboxylic acid ethyl ester. mp: 146°-149° C.

후처리

  1. temperaturethe mixture was heated at 84°-89° C. for 2 hrs
  2. concentrationThe reaction mixture was concentrated in vacuo
  3. dissolutionthe residue was dissolved in chloroform
  4. washThe chloroform layer was washed with water
  5. customdried
  6. customThe residue obtained through evaporation of chloroform
  7. customwas recrystallized from ethyl ether

출처 및 근거

ORD 기록
ord-1532107dbffa44fda9a11e8418d196ea
출처 데이터셋
uspto-grants-1984_09
특허 번호
US04472579

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