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Dimethylamine → N,N-dimethyl-[6-[4-(2-methylbenzoyl)benzoyl]-4,5,6,7-tetrahydrofuro[2,3-c]pyridin-2-ylmethyl]amine

HRID 611271
ノート
印刷プレビュー

反応式

HRID 611271 の反応式
[CH3:1][C:2]1[CH:26]=[CH:25][CH:24]=[CH:23][C:3]=1[C:4]([C:6]1[CH:22]=[CH:21][C:9]([C:10]([N:12]2[CH2:17][CH2:16][C:15]3[CH:18]=[CH:19][O:20][C:14]=3[CH2:13]2)=[O:11])=[CH:8][CH:7]=1)=[O:5].[CH3:27][NH:28][CH3:29].[CH2:30]=O>C(O)(=O)C>[CH3:27][N:28]([CH2:30][C:19]1[O:20][C:14]2[CH2:13][N:12]([C:10](=[O:11])[C:9]3[CH:21]=[CH:22][C:6]([C:4](=[O:5])[C:3]4[CH:23]=[CH:24][CH:25]=[CH:26][C:2]=4[CH3:1])=[CH:7][CH:8]=3)[CH2:17][CH2:16][C:15]=2[CH:18]=1)[CH3:29]
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

5

反応物 3

HCID 674DimethylamineHCID 712FormaldehydeHCID 196000596-[4-(2-Methylbenzoyl)benzoyl]-4,5,6,7-tetrahydrofuro[2,3-c]pyridine

生成物 1

HCID 19599918N,N-dimethyl-[6-[4-(2-methylbenzoyl)benzoyl]-4,5,6,7-tetrahydrofuro[2,3-c]pyridin-2-ylmethyl]amine

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 0.250 g (0.724 mmol) of 6-[4-(2-methylbenzoyl)benzoyl]-4,5,6,7-tetrahydrofuro[2,3-c]pyridine in 10 ml of acetic acid, 0.098 ml (1.09 mmol) of 50% aqueous dimethylamine and 0.088 ml (1.09 mmol) of 37% aqueous formaldehyde were added, followed by stirring at 100° C. for 120 minutes. After the solvent was distilled off under reduced pressure, the residual solution was alkalified with 5% aqueous sodium hydrogen carbonate and extracted with dichloromethane 2 times. The combined organic layer was washed with water and dried over anhydrous magnesium sulfate; the solvent was distilled off under reduced pressure. The resulting crude product was purified by silica gel column chromatography (ethyl acetate/methanol=5/1) to yield the desired product.

後処理

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

出典と根拠

ORDレコード
ord-17cf343580ad4c549c03b301eadace28
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

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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