Hydrochloric Acid → 1-(3-Acetylaminopropyl)-4-benzhydrylpiperazine

HRID 280854ノート

反応式

HRID 280854 の反応式
[NH2:1][CH2:2][CH2:3][CH2:4][N:5]1[CH2:10][CH2:9][N:8]([CH:11]([C:18]2[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=2)[C:12]2[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=2)[CH2:7][CH2:6]1.[C:24](OC(=O)C)(=[O:26])[CH3:25].Cl>>[C:24]([NH:1][CH2:2][CH2:3][CH2:4][N:5]1[CH2:6][CH2:7][N:8]([CH:11]([C:18]2[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=2)[C:12]2[CH:13]=[CH:14][CH:15]=[CH:16][CH:17]=2)[CH2:9][CH2:10]1)(=[O:26])[CH3:25]

参加物

4

反応物 3

HCID 313Hydrochloric AcidHCID 7918Acetic AnhydrideHCID 137677783-(4-Benzhydryl-1-piperazinyl)-1-propanamine

生成物 1

HCID 133628451-(3-Acetylaminopropyl)-4-benzhydrylpiperazine

反応条件

温度
100 °C

実験手順

A mixture of 1-(3-aminopropyl)-4-benzhydrylpiperazine (1.55 g) and acetic anhydride (16 ml) was stirred at 100° C. for 1.5 hours. The reaction mixture was concentrated and the residue was extracted with ethyl acetate. The extract was washed successively with aqueous sodium bicarbonate and water, dried and evaporated in vacuo. The residue was purified by column chromatography on silica gel eluting with ethyl acetate. The fractions containing the desired compound were combined and evaporated in vacuo to give a residue. According to a conventional manner, the residue was converted to hydrochloric acid salt, which was recrystallized from a mixture of methanol and diethyl ether to afford 1-(3-acetylaminopropyl)-4-benzhydrylpiperazine (0.8 g) as white crystals. mp: 240°-255° C. (dec.)

後処理

  1. concentrationThe reaction mixture was concentrated
  2. extractionthe residue was extracted with ethyl acetate
  3. washThe extract was washed successively with aqueous sodium bicarbonate and water
  4. customdried
  5. customevaporated in vacuo
  6. customThe residue was purified by column chromatography on silica gel eluting with ethyl acetate
  7. additionThe fractions containing the desired compound
  8. customevaporated in vacuo
  9. customto give a residue
  10. customwas recrystallized from a mixture of methanol and diethyl ether

出典と根拠

ORDレコード
ord-a6f207cf2e004f3b945b0f31957d5aeb
出典データセット
uspto-grants-1986_05
特許番号
US04591590

反応ノート

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