3-Chloro-2-methylaniline → 1-(3-Chloro-2-methylphenyl)piperazine

HRID 75479

反応式

HRID 75479 の反応式
[Cl:1][C:2]1[C:3]([CH3:9])=[C:4]([CH:6]=[CH:7][CH:8]=1)[NH2:5].Cl.Cl[CH2:12][CH2:13][NH:14][CH2:15][CH2:16]Cl.C([O-])([O-])=O.[Na+].[Na+]>C(O)CCC>[Cl:1][C:2]1[C:3]([CH3:9])=[C:4]([N:5]2[CH2:16][CH2:15][NH:14][CH2:13][CH2:12]2)[CH:6]=[CH:7][CH:8]=1

参加物

5

反応物 3

HCID 68943-Chloro-2-methylaniline2 回HCID 10340Sodium CarbonateHCID 522769Bis(2-chloroethyl)amine hydrochloride2 回

生成物 1

HCID 38008451-(3-Chloro-2-methylphenyl)piperazine収率 81%

試薬・触媒・溶媒 1

HCID 2631-Butanol溶媒

実験手順

To a stirred solution of 3-chloro-2-methylaniline (compound 26, 21.6 g, 0.15 mol) in n-butanol (200 ml) was added bis(2-chloroethyl)amine hydrochloride (compound 27, 30 g, 0.17 mol) at room temperature and allowed to refluxed temperature for 2 days. After cooled to room temperature Na2CO3 (9 g, 0.08 mol) was added and then reaction mixture was refluxed 30 min. The resulting mixture was filtered with n-butanol (100 ml) and collected solid was dried under reduced pressure to be obtained title compound (24.8 g, 81%) as a white solid.

後処理

  1. temperatureto refluxed temperature for 2 days
  2. additionwas added
  3. customreaction mixture
  4. temperaturewas refluxed 30 min
  5. filtrationThe resulting mixture was filtered with n-butanol (100 ml)
  6. customcollected solid
  7. customwas dried under reduced pressure

出典と根拠

ORDレコード
ord-b47952b60a9140c5b2852192c775aefc
出典データセット
uspto-grants-2014_09
特許番号
US08835436B2

関連ノート

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