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Formaldehyde → HCID 19600068、化合物

HRID 611217
ノート
印刷プレビュー

反応式

HRID 611217 の反応式
C(O[C:6]([N:8]([CH2:17][CH2:18][CH2:19][CH2:20][CH2:21][CH2:22][C:23]1[CH:28]=[CH:27][CH:26]=[CH:25][CH:24]=1)[CH2:9][CH2:10][CH2:11][C:12]1[CH:16]=[CH:15][O:14][CH:13]=1)=O)(C)(C)C.C=O>C(O)(=O)C>[C:23]1([CH2:22][CH2:21][CH2:20][CH2:19][CH2:18][CH2:17][N:8]2[CH2:9][CH2:10][CH2:11][C:12]3[CH:16]=[CH:15][O:14][C:13]=3[CH2:6]2)[CH:28]=[CH:27][CH:26]=[CH:25][CH:24]=1
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 712FormaldehydeHCID 19600203HCID 19600203、化合物

生成物 1

HCID 19600068HCID 19600068、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 the above crude N-[3-(3-furyl)propyl]-6-phenylhexylamine in 100 ml of acetic acid, 0.74 g (9.1 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 3/1) 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 to 3/1)

出典と根拠

ORDレコード
ord-78f390fdd6754aaa82d6dc2a943939a5
出典データセット
uspto-grants-1999_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05998433

反応ノート

読み込み中…

このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート