Benzene → N-(4-(4-(Phenylmethyl)-1-piperazinyl)phenyl)acetamide

HRID 1533900

反応式

HRID 1533900 の反応式
[C:1]1([CH2:7][N:8]2[CH2:13][CH2:12][N:11]([C:14]3[CH:19]=[CH:18][C:17]([NH2:20])=[CH:16][CH:15]=3)[CH2:10][CH2:9]2)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.C(N(CC)CC)C.[C:28](Cl)(=[O:30])[CH3:29].C1C=CC=CC=1>C(OCC)(=O)C.[OH-].[Na+]>[C:1]1([CH2:7][N:8]2[CH2:9][CH2:10][N:11]([C:14]3[CH:15]=[CH:16][C:17]([NH:20][C:28](=[O:30])[CH3:29])=[CH:18][CH:19]=3)[CH2:12][CH2:13]2)[CH:2]=[CH:3][CH:4]=[CH:5][CH:6]=1

参加物

7

反応物 4

HCID 241BenzeneHCID 6367Acetyl chloride2 回HCID 8471TriethylamineHCID 7372594-(4-Benzylpiperazin-1-yl)aniline

生成物 1

HCID 960610N-(4-(4-(Phenylmethyl)-1-piperazinyl)phenyl)acetamide収率 104.5%

試薬・触媒・溶媒 2

HCID 8857Ethyl Acetate溶媒2 回HCID 14798Sodium Hydroxide溶媒

実験手順

To a solution of 8.5 g (0.03 mol) of 4-[4-(phenylmethyl)-1-piperazinyl]benzeneamine and 16.0 g (0.16 mol) of triethylamine in 450 mL of ethyl acetate was added, dropwise, a solution of 2.5 g (0.035 mol) of acetyl chloride in 50 mL of ethyl acetate. The mixture was magnetically stirred for 3 h and then heated at reflux for 1 h. The excess acetyl chloride was co-distilled with benzene and the resulting oil was shaken in 400 mL of 10% sodium hydroxide solution. The suspended tan solid was collected by filtration, washed thrice with 100 mL portions of water, and air dried to give 9.7 g (99%) of crude product. A one-gram portion was recrystallized from benzene/petroleum ether to give 100 mg of cream colored solid, mp 159°-161° C.

後処理

  1. temperatureheated
  2. temperatureat reflux for 1 h
  3. filtrationThe suspended tan solid was collected by filtration
  4. washwashed thrice with 100 mL portions of water, and air
  5. customdried

出典と根拠

ORDレコード
ord-b91b614deb55459cb6f1f80f11f2fd93
出典データセット
uspto-grants-1992_02
特許番号
US05086055

関連ノート

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