Nitric Acid → 2,2,2-Trichloro-1-(1-methyl-4-nitro-1H-pyrrol-2-yl)ethan-1-one

HRID 1831029노트

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HRID 1831029 반응식
C(OC(=O)C)(=O)C.[CH3:8][N:9]1[CH:13]=[CH:12][CH:11]=[C:10]1[C:14](=[O:19])[C:15]([Cl:18])([Cl:17])[Cl:16].[N+:20]([O-])([OH:22])=[O:21]>C(O)(C)C>[CH3:8][N:9]1[CH:13]=[C:12]([N+:20]([O-:22])=[O:21])[CH:11]=[C:10]1[C:14](=[O:19])[C:15]([Cl:16])([Cl:17])[Cl:18]

참가 물질

5

반응물 3

HCID 944Nitric AcidHCID 7918Acetic AnhydrideHCID 27771642,2,2-Trichloro-1-(1-methyl-1H-pyrrol-2-yl)-1-ethanone

생성물 1

HCID 27599662,2,2-Trichloro-1-(1-methyl-4-nitro-1H-pyrrol-2-yl)ethan-1-one수율 70%

시약·촉매·용매 1

HCID 3776Isopropanol용매

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온도
-40 °C

실험 절차

An acetic anhydride solution (200 ml) containing 3 (45.2 g, 0.200 mol) was cooled to −40° C., and then fuming nitric acid (18.5 ml, 0.360 mol) was dropped into the solution at the same temperature. After stirring the mixture for 2 hours at a room temperature, isopropanol was added to precipitate a solid. The precipitated solid was collected by filtration to obtain a nitro substance 5 (27.2 g). The filtrate was distilled under a reduced pressure, and the obtained residue was subjected to silica gel column chromatography to further obtain 5 (10.7 g) from an elusion position of ethyl acetate-hexane (1:10, v/v). (Total yield: 70%)

후처리

  1. customto precipitate a solid
  2. filtrationThe precipitated solid was collected by filtration

출처 및 근거

ORD 기록
ord-e3fc111ae3f845cfaf886ae48fab0e9e
출처 데이터셋
uspto-grants-2006_06
특허 번호
US07067622B2

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