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Bromine → HCID 15257067, 화합물

HRID 589047
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HRID 589047 반응식
[Br:1]Br.[CH3:3][CH:4]([CH3:13])[C:5]([C:7]1[CH:12]=[CH:11][CH:10]=[CH:9][N:8]=1)=[O:6]>C(O)(=O)C>[Br:1][C:4]([CH3:13])([CH3:3])[C:5]([C:7]1[CH:12]=[CH:11][CH:10]=[CH:9][N:8]=1)=[O:6]
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참가 물질

4

반응물 2

HCID 24408BromineHCID 101083Isopropyl 2-pyridyl ketone

생성물 1

HCID 15257067HCID 15257067, 화합물

시약·촉매·용매 1

HCID 176Acetic Acid용매2회

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온도
105 °C

실험 절차

Bromine (2.1 g, 13.4 mmol) dissolved in acetic acid (1 mL) was added slowly to a mixture of 2-methyl-(1-pyridin-2-yl)propan-1-one (2.0 g, 13 mmol) in acetic acid (20 mL) at room temperature. The reaction was heated to 105° C. for 3 h, allowed to cool to room temperature, and concentrated in vacuo to give a dark semisolid. The crude product was partitioned between ethyl acetate and saturated aqueous sodium bicarbonate. The combined organic layer was washed with brine, dried over magnesium sulfate, and concentrated to give 2-bromo-2-methyl-1-(pyridin-2-yl)propan-1-one as a very dark oil (3.0 g, 98%). LCMS calculated for C9H11BrNO (M+H)+: m/z=227.9, 229.9. found: 228.1, 230.1.

후처리

  1. temperatureto cool to room temperature
  2. concentrationconcentrated in vacuo
  3. customto give a dark semisolid
  4. customThe crude product was partitioned between ethyl acetate and saturated aqueous sodium bicarbonate
  5. washThe combined organic layer was washed with brine
  6. dry with materialdried over magnesium sulfate
  7. concentrationconcentrated

출처 및 근거

ORD 기록
ord-f2a6d89a5a294974a64d40c81ed4dd49
출처 데이터셋
uspto-grants-2016_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09227985B2

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