N-bromobutanimide → HCID 49766558, 화합물

HRID 418561노트

반응식

HRID 418561 반응식
[NH2:1][C:2]1[CH:7]=[CH:6][C:5]([N+:8]([O-:10])=[O:9])=[CH:4][C:3]=1[OH:11].C1C(=O)N([Br:19])C(=O)C1.C(OCC)(=O)C.CCCCCC>CC#N>[NH2:1][C:2]1[C:7]([Br:19])=[CH:6][C:5]([N+:8]([O-:10])=[O:9])=[CH:4][C:3]=1[OH:11]

참가 물질

5

반응물 3

HCID 67184N-bromobutanimideHCID 49847212-Amino-5-NitrophenolHCID 21226206Ethyl acetate hexane

생성물 1

HCID 49766558HCID 49766558, 화합물

시약·촉매·용매 1

HCID 6342Acetonitrile용매

실험 절차

A solution of 2-amino-5-nitrophenol (97, 24 g, 156 mmol) in CH3CN (1 L) was treated with NBS (28.8 g, 160.8 mmol) at room temperature. After stirring for 1 hour, the solvent was removed to afford brown precipitate, which was taken up with ethyl acetate:hexane (1:1). The precipitate was filtered and was used for the next step without further purification (33 g, 91%). A small amount of sample was purified by column chromatography on silica gel for analysis; 1H NMR (500 MHz, CD3OD): δ 4.93 (brs, 3H), 7.50 (d, 1H, J=2.4 Hz), 7.89 (d, 1H, J=2.4 Hz); 13C NMR (125 MHz, CD3OD): δ 105.5, 108.7, 121.8, 138.5, 143.7, 144.8; HRMS (FAB) calcd for C6H5BrN2O3(M+) 231.9484. found 231.9479.

후처리

  1. customthe solvent was removed
  2. customto afford brown precipitate, which
  3. filtrationThe precipitate was filtered
  4. customwas used for the next step without further purification (33 g, 91%)
  5. customA small amount of sample was purified by column chromatography on silica gel for analysis

출처 및 근거

ORD 기록
ord-d59f48a27e5b4d25a5d894b43a356078
출처 데이터셋
uspto-grants-2012_01
특허 번호
US08093287B2

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