Formaldehyde → HCID 19600111、化合物

HRID 611240ノート

反応式

HRID 611240 の反応式
[CH2:1]([NH:8][CH2:9][CH2:10][C:11]1[CH:15]=[CH:14][O:13][CH:12]=1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[CH2:16]=O>C(O)(=O)C>[CH2:1]([N:8]1[CH2:9][CH2:10][C:11]2[CH:15]=[CH:14][O:13][C:12]=2[CH2:16]1)[C:2]1[CH:3]=[CH:4][CH:5]=[CH:6][CH:7]=1

参加物

4

反応物 2

HCID 712FormaldehydeHCID 19600250HCID 19600250、化合物

生成物 1

HCID 19600111HCID 19600111、化合物

試薬・触媒・溶媒 1

HCID 176Acetic Acid溶媒

反応条件

温度
100 °C

実験手順

To a solution of 5.603 g (27.838 mmol) of N-benzyl-2-(3-furyl)ethylamine in 50 ml of acetic acid, 2.71 g (33.4 mmol) of 37% aqueous formaldehyde was added, followed by stirring at 100° C. for 1 hour. After the solvent was distilled off under reduced pressure, the residual solution was alkalified with aqueous sodium hydroxide and extracted with dichloromethane 3 times. The combined organic layer was dried over anhydrous magnesium sulfate; the solvent was distilled off under reduced pressure. The resulting crude product was purified by silica gel column chromatography (hexane/ethyl acetate=9/1) to yield the desired product.

後処理

  1. distillationAfter the solvent was distilled off under reduced pressure
  2. extractionextracted with dichloromethane 3 times
  3. dry with materialThe combined organic layer was dried over anhydrous magnesium sulfate
  4. distillationthe solvent was distilled off under reduced pressure
  5. customThe resulting crude product was purified by silica gel column chromatography (hexane/ethyl acetate=9/1)

出典と根拠

ORDレコード
ord-5fbee235727342598dcf324d0864cc4c
出典データセット
uspto-grants-1999_12
特許番号
US05998433

反応ノート

読み込み中…