Sodium hydride → HCID 9282035, 화합물

HRID 373075노트

반응식

HRID 373075 반응식
[NH2:1][C:2]1[CH:15]=[CH:14][C:5]([C:6]([C:8]2[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=2)=[O:7])=[CH:4][C:3]=1[N+:16]([O-:18])=[O:17].[CH3:19][O:20][C:21]1[CH:28]=[CH:27][C:24]([CH2:25]Cl)=[CH:23][CH:22]=1.[H-].[Na+].[Cl-].[NH4+]>CN(C)C=O.C(OCC)(=O)C>[CH3:19][O:20][C:21]1[CH:28]=[CH:27][C:24]([CH2:25][NH:1][C:2]2[CH:15]=[CH:14][C:5]([C:6]([C:8]3[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=3)=[O:7])=[CH:4][C:3]=2[N+:16]([O-:18])=[O:17])=[CH:23][CH:22]=1

참가 물질

7

반응물 4

HCID 24758Sodium hydrideHCID 25517Ammonium ChlorideHCID 699934-Methyloxybenzyl chlorideHCID 5969704-Amino-3-nitrobenzophenone

생성물 1

HCID 9282035HCID 9282035, 화합물수율 59.2%

시약·촉매·용매 2

HCID 6228Dimethylformamide용매HCID 8857Ethyl Acetate용매

실험 절차

To a solution of 2.20 g of 4-amino-3-nitrobenzophenone and 1.57 g of 4-methoxybenzyl chloride in 25 ml of N,N-dimethylformamide was added at room temperature 0.40 g of 60% dispersion of sodium hydride in mineral oil, and the mixture was stirred overnight. After addition of saturated ammonium chloride aqueous solution was completed, the reaction mixture diluted with ethyl acetate was washed with brine. Removal of the solvent under reduced pressure gave the crude product, which was chromatographed on silica gel. Elution with hexane-ethyl acetate (3:1) provided 1.95 g of 4-(4-methoxybenzylamino)-3-nitrobenzophenone.

후처리

  1. washwas washed with brine
  2. customRemoval of the solvent under reduced pressure
  3. customgave the crude product, which
  4. customwas chromatographed on silica gel
  5. washElution with hexane-ethyl acetate (3:1)

출처 및 근거

ORD 기록
ord-8f182f4d8a2c4bd5b51fa351e40d802c
출처 데이터셋
uspto-grants-1992_11
특허 번호
US05162318

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