N-methyl-2-pyrrolidone → 6,6'-Dimethyl-2,2',3',4'-tetramethoxy-5-trifluoromethyl-benzophenone

HRID 611719노트

반응식

HRID 611719 반응식
Br[C:2]1[CH:3]=[CH:4][C:5]([O:24][CH3:25])=[C:6]([C:22]=1[CH3:23])[C:7]([C:9]1[C:14]([CH3:15])=[CH:13][C:12]([O:16][CH3:17])=[C:11]([O:18][CH3:19])[C:10]=1[O:20][CH3:21])=[O:8].[F:26][C:27]([F:32])([F:31])C([O-])=O.[Na+].CN1CCCC1=O>CCOCC.O.[Cu]I>[CH3:23][C:22]1[C:6]([C:7]([C:9]2[C:14]([CH3:15])=[CH:13][C:12]([O:16][CH3:17])=[C:11]([O:18][CH3:19])[C:10]=2[O:20][CH3:21])=[O:8])=[C:5]([O:24][CH3:25])[CH:4]=[CH:3][C:2]=1[C:27]([F:32])([F:31])[F:26]

참가 물질

7

반응물 3

HCID 13387N-methyl-2-pyrrolidoneHCID 517019Sodium TrifluoroacetateHCID 6451057Metrafenone

생성물 1

HCID 226713936,6'-Dimethyl-2,2',3',4'-tetramethoxy-5-trifluoromethyl-benzophenone

시약·촉매·용매 3

HCID 24350Copper(1+) iodide; Copper(I) iodide; Cuprous iodide; Cuprous iodide (CuI)촉매HCID 962Water용매HCID 3283Diethyl Ether용매

반응 조건

온도
160 °C

실험 절차

A mixture of 63C (6.15 g, 0.015 mol), sodium trifluoroacetate (9.52 g, 0.07 mol), copper-(I)iodide (13.37 g, 0.07 mol) and 1-N-methyl-2-pyrrolidinone (100 ml) is heated to 160° C. for 118 hours. The reaction mixture is cooled to room temperature and diluted with ether and water. The organic phase is separated and concentrated and the residue is purified by column chromatography (petrol ether:ethyl acetate, 95:5 v/v) yielding the pure product as white crystals, 1.3 g, (22%) having a melting point of 95-96° C.

후처리

  1. temperatureThe reaction mixture is cooled to room temperature
  2. customThe organic phase is separated
  3. concentrationconcentrated
  4. customthe residue is purified by column chromatography (petrol ether:ethyl acetate, 95:5 v/v)

출처 및 근거

ORD 기록
ord-ce0e17e919c2490d9f747aa244f6f4a0
출처 데이터셋
uspto-grants-1999_12
특허 번호
US06001883

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