Acetone → HCID 14839595、化合物

HRID 1031582ノート

反応式

HRID 1031582 の反応式
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]

参加物

7

反応物 4

HCID 180AcetoneHCID 6343EthanethiolHCID 11430Potassium CarbonateHCID 11844477HCID 11844477、化合物

生成物 1

HCID 14839595HCID 14839595、化合物収率 79%

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 8857Ethyl Acetate溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-a52c8384d56146a98e135509a451ec0a
出典データセット
uspto-grants-1990_09
特許番号
US04954507

反応ノート

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