1-Methylpiperazine → 1-[(3-Bromophenyl)(4-chlorophenyl)methyl]-4-methylpiperazine

HRID 845219ノート

反応式

HRID 845219 の反応式
[Br:1][C:2]1[CH:3]=[C:4]([CH:14]=[CH:15][CH:16]=1)[CH:5](Cl)[C:6]1[CH:11]=[CH:10][C:9]([Cl:12])=[CH:8][CH:7]=1.[CH3:17][N:18]1[CH2:23][CH2:22][NH:21][CH2:20][CH2:19]1>C(Cl)Cl>[Br:1][C:2]1[CH:3]=[C:4]([CH:14]=[CH:15][CH:16]=1)[CH:5]([N:21]1[CH2:22][CH2:23][N:18]([CH3:17])[CH2:19][CH2:20]1)[C:6]1[CH:11]=[CH:10][C:9]([Cl:12])=[CH:8][CH:7]=1

参加物

4

反応物 2

HCID 531671-MethylpiperazineHCID 201324411-Bromo-3-[chloro(4-chlorophenyl)methyl]benzene

生成物 1

HCID 189559271-[(3-Bromophenyl)(4-chlorophenyl)methyl]-4-methylpiperazine

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

The benzhydryl chloride from above (8.33 g, 26.4 mmol) in 10 mL of N-methylpiperazine was heated to 110° for 12 hours under nitrogen. After cooling to room temperature, the residue was dissolved in 75 mL of methylene chloride and washed with 40 mL of 1M sodium hydroxide and two 50 mL portions of water. After drying over sodium sulfate, the solvent was removed in vacuo to give 10.2 g of 1-(3-bromo-4'-chlorobenzhydryl)-4-methylpiperazine as a dark oil. A portion of the oil was dissolved in ether and converted to the dihydrochloride salt with ethanolic hydrogen chloride. Recrystallization from 2:1 ethanol:methanol gave white powdery crystals, m.p. 229°-231°. Calc. for C18H20BrClN2.2HCl: C, 47.76; H, 4.90; N, 6.19. Found: C, 47.55; H, 4.91; N, 6.13.

後処理

  1. washwashed with 40 mL of 1M sodium hydroxide and two 50 mL portions of water
  2. dry with materialAfter drying over sodium sulfate
  3. customthe solvent was removed in vacuo

出典と根拠

ORDレコード
ord-aab322f587a5440d9c69f40eada708ff
出典データセット
uspto-grants-1988_07
特許番号
US04757074

反応ノート

読み込み中…