Acetone → HCID 14839595, 화합물

HRID 1031582노트

반응식

HRID 1031582 반응식
CC(C)=O.[CH2:5]([O:7][C:8]([C:10]1[C:19](=[O:20])[C:18]2[C:13](=[N:14][C:15](Cl)=[C:16]([F:21])[CH:17]=2)[N:12]([C:23]([CH3:26])([CH3:25])[CH3:24])[CH:11]=1)=[O:9])[CH3:6].C(=O)([O-])[O-].[K+].[K+].[CH2:33]([SH:35])[CH3:34]>O.C(OC(=O)C)C>[CH2:5]([O:7][C:8]([C:10]1[C:19](=[O:20])[C:18]2[C:13](=[N:14][C:15]([S:35][CH2:33][CH3:34])=[C:16]([F:21])[CH:17]=2)[N:12]([C:23]([CH3:26])([CH3:25])[CH3:24])[CH:11]=1)=[O:9])[CH3:6]

참가 물질

7

반응물 4

HCID 180AcetoneHCID 6343EthanethiolHCID 11430Potassium CarbonateHCID 11844477HCID 11844477, 화합물

생성물 1

HCID 14839595HCID 14839595, 화합물수율 79%

시약·촉매·용매 2

HCID 962Water용매HCID 8857Ethyl Acetate용매

실험 절차

Acetone (90 mL) was added to a mixture of 1.96 g (6 mmoles) of 6-fluoro-7-chloro-1-(1,1-dimethylethyl)-1,4-dihydro-4-oxo-1,8-naphthyridine-3-carboxylic acid ethyl ester and 2.5 g (18 mmoles) of anhydrous potassium carbonate. To this suspension was added 1.33 mL (18 mmoles) of ethanethiol. After heating to reflux for 2.5 hours, the solvent was eliminated in vacuo. The residue was taken up with ethylacetate and water. The organic layer was separated, washed with water and brine, and dried over magnesium sulfate. The resulting solid was treated with ether to give 1.67 g of titled compound. MP 159°-60° C.

후처리

  1. temperatureAfter heating
  2. temperatureto reflux for 2.5 hours
  3. customThe organic layer was separated
  4. washwashed with water and brine
  5. dry with materialdried over magnesium sulfate
  6. additionThe resulting solid was treated with ether

출처 및 근거

ORD 기록
ord-a52c8384d56146a98e135509a451ec0a
출처 데이터셋
uspto-grants-1990_09
특허 번호
US04954507

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