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2-(2-Bromo-4-nitrophenyl)acetic acid → HCID 12404389, 화합물

HRID 2173392
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HRID 2173392 반응식
[Br:1][C:2]1[CH:7]=[C:6]([N+:8]([O-])=O)[CH:5]=[CH:4][C:3]=1[CH2:11][C:12]([OH:14])=[O:13]>[OH-].[NH4+].O>[NH2:8][C:6]1[CH:5]=[CH:4][C:3]([CH2:11][C:12]([OH:14])=[O:13])=[C:2]([Br:1])[CH:7]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 1

HCID 124043882-(2-Bromo-4-nitrophenyl)acetic acid

생성물 1

HCID 12404389HCID 12404389, 화합물

시약·촉매·용매 2

HCID 962Water용매HCID 14923Ammonium Hydroxide용매

실험 절차

A solution of (2-bromo-4-nitrophenyl)acetic acid (500 mg, 2 mmol) in 11 mL of concentrated ammonium hydroxide was added a solution of FeSO4.7H2O (3.4 g, 12 mmol) in 11 mL of water over 5 minutes, and then the mixture was heated to reflux for 1 hour. Cooled to ambient temperature, filtered off solids and the filtrate was adjusted to pH to 5 with 2N HCl. Extracted with EtOAc and combined organic layers were washed with water, dried over anhydrous sodium sulfate, and concentrated to get (4-amino-2-bromophenyl)acetic acid. 1H-NMR (300 MHz, CDCl3) δ ppm 7.01 (d, J=8.0 Hz, 1H), 6.92 (d, J=2.0 Hz, 1H), 6.62 (dd, J=2.5 Hz, 1H), 3.61 (s, 2H).

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후처리

  1. temperaturethe mixture was heated
  2. temperatureto reflux for 1 hour
  3. filtrationfiltered off solids
  4. extractionExtracted with EtOAc
  5. washwere washed with water
  6. dry with materialdried over anhydrous sodium sulfate
  7. concentrationconcentrated

출처 및 근거

ORD 기록
ord-953dc95a5762439fb61d8f5fe8a545d2
출처 데이터셋
uspto-grants-2015_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09056859B2

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