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

HRID 1464666

反応式

HRID 1464666 の反応式
[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]

参加物

6

反応物 3

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

生成物 1

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

試薬・触媒・溶媒 2

HCID 3283Diethyl Ether溶媒2 回HCID 8857Ethyl Acetate溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-9d1f87d5eba44bb3b33d4bc1ab6d5b5d
出典データセット
uspto-grants-1994_04
特許番号
US05306827

関連ノート

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