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

HRID 481347

반응식

HRID 481347 반응식
[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]

참가 물질

5

반응물 3

HCID 6577Chloroacetyl chlorideHCID 10112Calcium CarbonateHCID 919652-Mepp

생성물 1

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

시약·촉매·용매 1

HCID 6569Methyl Ethyl Ketone용매

반응 조건

온도
0 °C

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-6f100b1ebd584b75824b3201336f9e84
출처 데이터셋
uspto-grants-1998_08
특허 번호
US05789412

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