Sodium Hydroxide → HCID 12138351、化合物

HRID 1271666ノート

反応式

HRID 1271666 の反応式
[CH3:1][N:2]([CH3:22])[C:3]([S:5][C:6]1[CH:7]=[C:8]([CH:13]=[C:14]([S:16][C:17](=[O:21])[N:18]([CH3:20])[CH3:19])[CH:15]=1)[C:9]([O:11]C)=[O:10])=[O:4].[OH-].[Na+]>>[CH3:1][N:2]([CH3:22])[C:3]([S:5][C:6]1[CH:7]=[C:8]([CH:13]=[C:14]([S:16][C:17](=[O:21])[N:18]([CH3:20])[CH3:19])[CH:15]=1)[C:9]([OH:11])=[O:10])=[O:4]

参加物

3

反応物 2

HCID 14798Sodium HydroxideHCID 12138342Methyl 3,5-bis(dimethylcarbamoylthio)benzoate

生成物 1

HCID 12138351HCID 12138351、化合物収率 87.2%

実験手順

Methyl 3,5-bis(dimethylcarbamoylthio)benzoate (3.42 g, 10 mmol) was made to react with 5% aqueous sodium hydroxide solution (10 ml. 12.5 mmol) for 3 hours at 22–25° C. with stirring. After cooling by the addition of 50 ml of ice-water, the reaction mixture was extracted with ethyl acetate (300 ml×3) and the extract was dried over magnesium sulfate. The ethyl acetate was evaporated under reduced pressure and the colorless crystals thus obtained was recrystallized from ethanol to give 2.86 g (87.2%) of 3,5-bis(dimethylcarbamoylthio)benzoic acid as colorless needles. The melting point is 196–198° C. (with decomposition).

後処理

  1. extractionthe reaction mixture was extracted with ethyl acetate (300 ml×3)
  2. dry with materialthe extract was dried over magnesium sulfate
  3. customThe ethyl acetate was evaporated under reduced pressure
  4. customthe colorless crystals thus obtained
  5. customwas recrystallized from ethanol

出典と根拠

ORDレコード
ord-f664399a9bc0413e9379e3c931517d37
出典データセット
uspto-grants-2007_04
特許番号
US07205428B2

反応ノート

読み込み中…