Potassium Carbonate → HCID 82810771, 화합물

HRID 404216

반응식

HRID 404216 반응식
[C:1](=O)([O-])[O-].[K+].[K+].CC(C)C(=O)C(P(=O)([O-])[O-])=[N+]=[N-].[F:19][C:20]1[C:27]([O:28][CH3:29])=[CH:26][CH:25]=[CH:24][C:21]=1[CH:22]=O>CO>[C:22]([C:21]1[CH:24]=[CH:25][CH:26]=[C:27]([O:28][CH3:29])[C:20]=1[F:19])#[CH:1]

참가 물질

5

반응물 3

HCID 11430Potassium CarbonateHCID 37744632-Fluoro-3-methoxybenzaldehydeHCID 86586111Dimethyl-1-diazo-2-oxopropylphosphonate

생성물 1

HCID 82810771HCID 82810771, 화합물수율 92.2%

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

Potassium carbonate (3.6 g, 26.0 mmol) and dimethyl-1-diazo-2-oxopropylphosphonate (2.4 mL, 15.6 mmol) were added sequentially to a solution of 2-fluoro-3-methoxybenzaldehyde (2.0 g, 13.0 mmol) in methanol (100 mL), and the reaction was allowed to stir at room temperature for 16 h. After concentrating the reaction mixture under reduced pressure, the crude material was purified by flash chromatography (40 g silica gel column, 0-40% gradient ethyl acetate in hexanes) to provide a clear colorless oil (1.8 g, 92%). MS (GCMS) m/z 150. 1H NMR (400 MHz, CHLOROFORM-d) δ3.31 (d, J=0.78 Hz, 1H) 3.90 (s, 3H) 6.93-7.11 (m, 3H).

후처리

  1. concentrationAfter concentrating the reaction mixture under reduced pressure
  2. customthe crude material was purified by flash chromatography (40 g silica gel column, 0-40% gradient ethyl acetate in hexanes)

출처 및 근거

ORD 기록
ord-0ee9c85b54f14a6d9bf2444ee02b6e73
출처 데이터셋
uspto-grants-2014_06
특허 번호
US08748466B2

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