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Ethanol → Unii-9tvu6uuo09

HRID 49528
ノート
印刷プレビュー

反応式

HRID 49528 の反応式
[C:1]([CH2:4][C:5]1[CH:6]=[CH:7][C:8]([O:25][CH3:26])=[C:9]([CH:24]=1)[C:10]([NH:12][CH2:13][C:14]1[CH:19]=[CH:18][C:17]([C:20]([F:23])([F:22])[F:21])=[CH:16][CH:15]=1)=[O:11])(=[O:3])N.C([OH:29])C.[OH-].[Na+].O>C(OCC)C>[CH3:26][O:25][C:8]1[CH:7]=[CH:6][C:5]([CH2:4][C:1]([OH:29])=[O:3])=[CH:24][C:9]=1[C:10](=[O:11])[NH:12][CH2:13][C:14]1[CH:19]=[CH:18][C:17]([C:20]([F:23])([F:22])[F:21])=[CH:16][CH:15]=1
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 4

HCID 702EthanolHCID 962WaterHCID 14798Sodium HydroxideHCID 120946625-carbamoylmethyl-2-methoxy-N-(4-trifluoromethylbenzyl)benzamide

生成物 1

HCID 9799335Unii-9tvu6uuo09

試薬・触媒・溶媒 1

HCID 3283Diethyl Ether溶媒

実験手順

To 700 mg of 5-carbamoylmethyl-2-methoxy-N-(4-trifluoromethylbenzyl)benzamide were added 21 ml of ethanol, 7 ml of 1 mol/l aqueous solution of sodium hydroxide, and the mixture was refluxed for 18 hours. The reaction mixture was poured into water, washed with ethyl acetate, and further the aqueous layer was adjusted to pH value of 1 to 2 with 2 mol/l hydrochloric acid, which was then extracted with ethyl acetate. The organic layer was washed with water and saturated brine in sequence and dried again over anhydrous sodium sulfate. Solvent was distilled off under reduced pressure, and the residue obtained was suspended with diethyl ether to collect the crystals by filtration. The crystals obtained were recrystallized from methylene chloride to obtain 435 mg of aimed product as colorless crystals.

後処理

  1. temperaturethe mixture was refluxed for 18 hours
  2. washwashed with ethyl acetate
  3. extractionwas then extracted with ethyl acetate
  4. washThe organic layer was washed with water and saturated brine in sequence
  5. dry with materialdried again over anhydrous sodium sulfate
  6. distillationSolvent was distilled off under reduced pressure
  7. customthe residue obtained
  8. customto collect the crystals
  9. filtrationby filtration
  10. customThe crystals obtained
  11. customwere recrystallized from methylene chloride

出典と根拠

ORDレコード
ord-8bbdcd7f42744919a823864bb298ee42
出典データセット
uspto-grants-2004_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06706763B1

反応ノート

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