Ethanol → HCID 68456339、化合物

HRID 500529

反応式

HRID 500529 の反応式
Cl.[CH3:2][C:3]1[CH:4]=[C:5]([NH:9][NH2:10])[CH:6]=[CH:7][CH:8]=1.C(O)C.[C:14]([OH:18])(=[O:17])[CH:15]=O>O>[C:3]1([CH3:2])[CH:8]=[CH:7][CH:6]=[C:5]([NH:9][N:10]=[CH:15][C:14]([OH:18])=[O:17])[CH:4]=1

参加物

5

反応物 3

HCID 702EthanolHCID 760Glyoxylic AcidHCID 71562m-Tolylhydrazinium(1+) chloride

生成物 1

HCID 68456339HCID 68456339、化合物収率 69%

試薬・触媒・溶媒 1

HCID 962Water溶媒3 回

反応条件

温度
60 °C

実験手順

3-Methylphenylhydrazine hydrochloride (15.9 g, 100 mmol) was dissolved in water (450 mL) and ethanol (600 mL) with heating at 60° C. A solution of glyoxylic acid (9.21 g, 100 mmol) in water (100 mL) was added to the warm solution using water (3×15 mL) to rinse. The reaction mixture was stirred at 60° C. for 45 minutes and then cooled slightly and concentrated to remove ethanol. The aqueous mixture was neutralized with NaOH and then water was added (800 mL). The precipitate was filtered, washed with water (3×100 mL), washed with hexanes (100 mL) and dried to give the subtitle compound as a brown solid (12.2 g, 69%).

後処理

  1. washto rinse
  2. temperaturecooled slightly
  3. concentrationconcentrated
  4. customto remove ethanol
  5. additionwater was added (800 mL)
  6. filtrationThe precipitate was filtered
  7. washwashed with water (3×100 mL)
  8. washwashed with hexanes (100 mL)
  9. customdried

出典と根拠

ORDレコード
ord-9a2a39e92d094dbda476973e38335bed
出典データセット
uspto-grants-2010_08
特許番号
US07772235B2

関連ノート

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