Chloroacetyl chloride → 2-Chloro-1-(4-o-tolylpiperazin-1-yl)ethanone

HRID 481347

反応式

HRID 481347 の反応式
[Cl:1][CH2:2][C:3](Cl)=[O:4].[C:6]1([CH3:18])[CH:11]=[CH:10][CH:9]=[CH:8][C:7]=1[N:12]1[CH2:17][CH2:16][NH:15][CH2:14][CH2:13]1.C(=O)([O-])[O-].[Ca+2]>C(C(C)=O)C>[Cl:1][CH2:2][C:3]([N:15]1[CH2:16][CH2:17][N:12]([C:7]2[CH:8]=[CH:9][CH:10]=[CH:11][C:6]=2[CH3:18])[CH2:13][CH2:14]1)=[O:4]

参加物

5

反応物 3

HCID 6577Chloroacetyl chlorideHCID 10112Calcium CarbonateHCID 919652-Mepp

生成物 1

HCID 47412122-Chloro-1-(4-o-tolylpiperazin-1-yl)ethanone収率 83%

試薬・触媒・溶媒 1

HCID 6569Methyl Ethyl Ketone溶媒

反応条件

温度
0 °C

実験手順

Chloroacetyl chloride (4.5 ml, 56.6 mmol) is added dropwise to a solution of 1-o-tolylpiperazine (8.31 [lacuna], 47.2 mmol) and calcium carbonate (14.2 g, 142 mmol) in methyl ethyl ketone (100 ml) cooled to 0° C. The reaction mixture is stirred at this temperature for 1 h 30 and is then filtered through Celite. The Celite is rinsed several times with ethyl acetate and 3M sodium hydroxide solution. The two phases of the filtrate are then separated and the organic phase is dried over magnesium sulfate, filtered and concentrated to give the expected product in the form of a brown solid.

後処理

  1. filtrationis then filtered through Celite
  2. washThe Celite is rinsed several times with ethyl acetate and 3M sodium hydroxide solution
  3. customThe two phases of the filtrate are then separated
  4. dry with materialthe organic phase is dried over magnesium sulfate
  5. filtrationfiltered
  6. concentrationconcentrated

出典と根拠

ORDレコード
ord-6f100b1ebd584b75824b3201336f9e84
出典データセット
uspto-grants-1998_08
特許番号
US05789412

関連ノート

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