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

HRID 2364781

반응식

HRID 2364781 반응식
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]

참가 물질

7

반응물 4

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

생성물 1

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

시약·촉매·용매 2

HCID 3007855Zincchloride촉매HCID 241Benzene용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-108a162284974588bcea8ba907eebf9d
출처 데이터셋
uspto-grants-2014_04
특허 번호
US08691938B2

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