Trichloroacetyl chloride → 5-(p-Chlorophenyl)pyrrol-5-yl trichloromethyl ketone

HRID 1464666노트

반응식

HRID 1464666 반응식
[Cl:1][C:2]([Cl:7])([Cl:6])[C:3](Cl)=[O:4].[Cl:8][C:9]1[CH:14]=[CH:13][C:12]([C:15]2[NH:16][CH:17]=[CH:18][CH:19]=2)=[CH:11][CH:10]=1.C(=O)([O-])[O-].[K+].[K+]>CCOCC.C(OCC)(=O)C>[Cl:1][C:2]([C:3]([C:15]1([C:12]2[CH:13]=[CH:14][C:9]([Cl:8])=[CH:10][CH:11]=2)[N:16]=[CH:17][CH:18]=[CH:19]1)=[O:4])([Cl:7])[Cl:6]

참가 물질

6

반응물 3

HCID 6420Trichloroacetyl chlorideHCID 11430Potassium CarbonateHCID 2724282-(4-Chlorophenyl)-1h-pyrrole

생성물 1

HCID 189303945-(p-Chlorophenyl)pyrrol-5-yl trichloromethyl ketone수율 77.7%

시약·촉매·용매 2

HCID 3283Diethyl Ether용매2회HCID 8857Ethyl Acetate용매

실험 절차

A solution of trichloroacetyl chloride (11.26 g, 0.0619 mol) in ether is treated with a solution of 2-(p-chlorophenyl)pyrrole (10.0 g, 0.0503 mol) in ether, stirred for four hours at room temperature, treated with saturated potassium carbonate solution and diluted with ethyl acetate. The organic phase is separated, washed with brine, dried over anhydrous magnesium sulfate and concentrated in vacuo to obtain a yellow solid. The solid is recrystallized from 2-propanol to give the title product as a yellow solid (12.63 g, mp 166°-168° C.) which is identified by 1HNMR spectral analysis.

후처리

  1. customThe organic phase is separated
  2. washwashed with brine
  3. dry with materialdried over anhydrous magnesium sulfate
  4. concentrationconcentrated in vacuo
  5. customto obtain a yellow solid
  6. customThe solid is recrystallized from 2-propanol

출처 및 근거

ORD 기록
ord-9d1f87d5eba44bb3b33d4bc1ab6d5b5d
출처 데이터셋
uspto-grants-1994_04
특허 번호
US05306827

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