tert-Butanol → 1,4-Bis(4-chloro-3-nitrophenyl)butane-1,4-dione

HRID 2364781

反応式

HRID 2364781 の反応式
C(NCC)C.C(O)(C)(C)C.[Cl:11][C:12]1[CH:17]=[CH:16][C:15]([C:18](=[O:20])[CH3:19])=[CH:14][C:13]=1[N+:21]([O-:23])=[O:22].Br[CH2:25][C:26]([C:28]1[CH:33]=[CH:32][C:31]([Cl:34])=[C:30]([N+:35]([O-:37])=[O:36])[CH:29]=1)=[O:27]>C1C=CC=CC=1.[Cl-].[Zn+2].[Cl-]>[Cl:11][C:12]1[CH:17]=[CH:16][C:15]([C:18](=[O:20])[CH2:19][CH2:25][C:26]([C:28]2[CH:33]=[CH:32][C:31]([Cl:34])=[C:30]([N+:35]([O-:37])=[O:36])[CH:29]=2)=[O:27])=[CH:14][C:13]=1[N+:21]([O-:23])=[O:22]

参加物

7

反応物 4

HCID 6386tert-ButanolHCID 8021DiethylamineHCID 795964'-Chloro-3'-nitroacetophenoneHCID 27783302-Bromo-1-(4-chloro-3-nitrophenyl)ethan-1-one

生成物 1

HCID 866490991,4-Bis(4-chloro-3-nitrophenyl)butane-1,4-dione

試薬・触媒・溶媒 2

HCID 3007855Zincchloride触媒HCID 241Benzene溶媒

実験手順

Zinc chloride (27.4 g, 201 mmol), diethylamine (15.6 mL, 151 mmol) and t-butanol (14.4 mL, 151 mmol) were combined in benzene (151 mL) at room temperature under a nitrogen atmosphere and stirred for 2 h. 1-(4-chloro-3-nitrophenyl)ethanone (30.1 g, 151 mmol) and 2-bromo-1-(4-chloro-3-nitrophenyl)ethanone (28 g, 101 mmol) were added. The mixture was stirred vigorously for 20 h, and the solid product was collected by filteration and rinsed with benzene, water, methanol, and dichloromethane. The solid was dried in a vacuum oven.

後処理

  1. stirringThe mixture was stirred vigorously for 20 h
  2. customthe solid product was collected by filteration
  3. washrinsed with benzene, water, methanol, and dichloromethane
  4. customThe solid was dried in a vacuum oven

出典と根拠

ORDレコード
ord-108a162284974588bcea8ba907eebf9d
出典データセット
uspto-grants-2014_04
特許番号
US08691938B2

関連ノート

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