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

HRID 611126
ノート
印刷プレビュー

反応式

HRID 611126 の反応式
[C:1]1([C:7]2[CH:23]=[CH:22][C:10]([C:11]([N:13]3[CH2:18][CH2:17][C:16]4[CH:19]=[CH:20][O:21][C:15]=4[CH2:14]3)=[O:12])=[CH:9][CH:8]=2)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.[CH3:24][NH:25][CH3:26].[CH2:27]=O>C(O)(=O)C>[CH3:24][N:25]([CH2:27][C:20]1[O:21][C:15]2[CH2:14][N:13]([C:11](=[O:12])[C:10]3[CH:9]=[CH:8][C:7]([C:1]4[CH:2]=[CH:3][CH:4]=[CH:5][CH:6]=4)=[CH:23][CH:22]=3)[CH2:18][CH2:17][C:16]=2[CH:19]=1)[CH3:26]
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 674Dimethylamine2 回HCID 712Formaldehyde2 回HCID 196000916-(4-Phenylbenzoyl)-4,5,6,7-tetrahydrofuro[2,3-c]pyridine

生成物 1

HCID 19600119N,N-dimethyl-[6-(4-phenylbenzoyl)-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 (0.824 mmol) of 6-(4-phenylbenzoyl)-4,5,6,7-tetrahydrofuro[2,3-c]pyridine in 20 ml of acetic acid, 0.112 ml (1.24 mmol) of 50% aqueous dimethylamine and 0.101 ml (1.24 mmol) of 37% aqueous formaldehyde were added, followed by stirring at 100° C. for 60 minutes. Additionally, 0.075 ml (0.82 mmol) of 50% aqueous dimethylamine and 0.067 ml (0.82 mmol) of 37% aqueous formaldehyde were added, followed by stirring for 20 minutes. After the solvent was distilled off under reduced pressure, the residual solution was alkalified with 5% aqueous solution of sodium hydrogen carbonate and extracted with dichloromethane 2 times. The combined organic layer was washed with water and dried over anhydrous sodium sulfate; the solvent was distilled off under reduced pressure. The resulting crude product was purified by silica gel column chromatography (chloroform to chloroform/methanol 50/1 to =25/1) to yield the desired product.

後処理

  1. stirringby stirring for 20 minutes
  2. distillationAfter the solvent was distilled off under reduced pressure
  3. extractionextracted with dichloromethane 2 times
  4. washThe combined organic layer was washed with water
  5. dry with materialdried over anhydrous sodium sulfate
  6. distillationthe solvent was distilled off under reduced pressure
  7. customThe resulting crude product was purified by silica gel column chromatography (chloroform to chloroform/methanol 50/1 to =25/1)

出典と根拠

ORDレコード
ord-07024860433a4981a0f4119d1a89b053
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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