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Hydrochloric Acid → HCID 15886891、化合物

HRID 651576
ノート
印刷プレビュー

反応式

HRID 651576 の反応式
[OH-].[K+].[CH:3]1[C:8]2[C:9]3[NH:10][C:11]4[C:16]([C:17]=3[CH:18]([C:20]([O:22]CC)=[O:21])[S:19][C:7]=2[CH:6]=[CH:5][CH:4]=1)=[CH:15][CH:14]=[CH:13][CH:12]=4.Cl>O.C(O)C>[CH:3]1[C:8]2[C:9]3[NH:10][C:11]4[C:16]([C:17]=3[CH:18]([C:20]([OH:22])=[O:21])[S:19][C:7]=2[CH:6]=[CH:5][CH:4]=1)=[CH:15][CH:14]=[CH:13][CH:12]=4
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 3

HCID 313Hydrochloric AcidHCID 14797Potassium HydroxideHCID 21709030HCID 21709030、化合物

生成物 1

HCID 15886891HCID 15886891、化合物収率 101.4%

試薬・触媒・溶媒 2

HCID 702Ethanol溶媒HCID 962Water溶媒

実験手順

A solution of 19.46 g of potassium hydroxide in 40 ml of water was added to a solution of 21.63 g of ethyl 6,11-dihydro-5-thia-11-aza-benzo[a]fluoren-6-carboxylate in 100 ml of ethanol. After reflux under heating for 2 hours, the reaction solution was adjusted to pH 3 with conc. hydrochloric acid, and extracted with ethyl acetate. The extract was washed with a saturated aqueous sodium chloride solution and dried over anhydrous sodium sulfate. After removal of the drying agent by filtration, the filtrate was concentrated under reduced pressure, and the residue was recrystallized from ethanol-hexane to give 19.94 g of 6,11-dihydro-5-thia-11-aza-benzo[a]fluoren-6-carboxylic acid.

後処理

  1. temperatureAfter reflux
  2. temperatureunder heating for 2 hours
  3. extractionextracted with ethyl acetate
  4. washThe extract was washed with a saturated aqueous sodium chloride solution
  5. dry with materialdried over anhydrous sodium sulfate
  6. customAfter removal of the drying agent
  7. filtrationby filtration
  8. concentrationthe filtrate was concentrated under reduced pressure
  9. customthe residue was recrystallized from ethanol-hexane

出典と根拠

ORDレコード
ord-fad3f20af3f5483f84f33d5f13404584
出典データセット
uspto-grants-2001_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06281355B1

反応ノート

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