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Methanol → HCID 22387885、化合物

HRID 1072816
ノート
印刷プレビュー

反応式

HRID 1072816 の反応式
[Cl:1][C:2]1[CH:23]=[C:22]([Cl:24])[CH:21]=[CH:20][C:3]=1[C:4]([C:6]1[C:7]2[CH:15]=[C:14]([C:16]([O:18]C)=[O:17])[CH:13]=[CH:12][C:8]=2[O:9][C:10]=1[CH3:11])=O.CO.[OH-].[Na+]>O1CCCC1>[C:16]([C:14]1[CH:13]=[CH:12][C:8]2[O:9][C:10]([CH3:11])=[C:6]([CH2:4][C:3]3[CH:20]=[CH:21][C:22]([Cl:24])=[CH:23][C:2]=3[Cl:1])[C:7]=2[CH:15]=1)([OH:18])=[O:17]
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 887MethanolHCID 14798Sodium HydroxideHCID 22388405HCID 22388405、化合物

生成物 1

HCID 22387885HCID 22387885、化合物

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

A mixture of 3-(2,4-dichlorobenzoyl)-5-(methoxycarbonyl)-2-methylbenzo[b]furan (0.57 g, 1.6 mmol), methanol (6 ml), tetrahydrofuran (6 ml) and a 2M aqueous sodium hydroxide solution (8.5 ml) was refluxed under heating for 40 min. The reaction mixture was concentrated under reduced pressure and water was added to the residue. The mixture was acidified with 3N hydrochloric acid and the precipitated solid was extracted with hot ethyl acetate. The organic layer was washed with saturated brine, and dried over anhydrous magnesium sulfate. The desiccant was filtered off and the filtrate was concentrated under reduced pressure to give the objective compound (0.54 g, quantitative) as colorless crystals.

後処理

  1. temperatureunder heating for 40 min
  2. concentrationThe reaction mixture was concentrated under reduced pressure and water
  3. additionwas added to the residue
  4. extractionthe precipitated solid was extracted with hot ethyl acetate
  5. washThe organic layer was washed with saturated brine
  6. dry with materialdried over anhydrous magnesium sulfate
  7. filtrationThe desiccant was filtered off
  8. concentrationthe filtrate was concentrated under reduced pressure
  9. customto give the objective compound (0.54 g, quantitative) as colorless crystals

出典と根拠

ORDレコード
ord-a036cf9fb5334e309c1f62ab1eeb10eb
出典データセット
uspto-grants-2005_06
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06911469B2

反応ノート

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