Potassium Carbonate → HCID 18455594, 화합물

HRID 1966312노트

반응식

HRID 1966312 반응식
[CH3:1][C@H:2]1[O:7][C@@H:6]([CH3:8])[CH2:5][NH:4][CH2:3]1.[Br:9][C:10]1[C:17]([N+:18]([O-:20])=[O:19])=[CH:16][C:13]([CH:14]=[O:15])=[C:12](F)[CH:11]=1.C(=O)([O-])[O-].[K+].[K+].CC(OC)(C)C>C(#N)C>[Br:9][C:10]1[C:17]([N+:18]([O-:20])=[O:19])=[CH:16][C:13]([CH:14]=[O:15])=[C:12]([N:4]2[CH2:5][CH:6]([CH3:8])[O:7][CH:2]([CH3:1])[CH2:3]2)[CH:11]=1

참가 물질

6

반응물 4

HCID 11430Potassium CarbonateHCID 15413tert-Butyl methyl etherHCID 6415002,6-Dimethylmorpholine, cis-HCID 184555954-Bromo-2-fluoro-5-nitrobenzaldehyde

생성물 1

HCID 18455594HCID 18455594, 화합물수율 63.6%

시약·촉매·용매 1

HCID 6342Acetonitrile용매

실험 절차

A solution of cis-2,6-dimethylmorpholine (1.06 g, 9.20 mmol) in acetonitrile (40 mL) is added to a flask containing 4-bromo-2-fluoro-5-nitrobenzaldehyde (from Step 1) (2.0 g, 8.06 mmol) and potassium carbonate (3.92 g, 28.4 mmol). The resulting slurry is stirred at room temperature for 63 hours. The mixture is poured into MTBE (100 mL) and is washed with water (100 mL) followed by brine (100 mL). The organics are filtered through silica gel and concentrated to give 1.76 g of bright yellow solid. 1H NMR (DMSO-d6) δ 9.93, 8.44, 7.53, 3.74-3.81, 3.48, 2.78, 1.12.

후처리

  1. washis washed with water (100 mL)
  2. filtrationThe organics are filtered through silica gel
  3. concentrationconcentrated

출처 및 근거

ORD 기록
ord-879672e9785b48c9ad9a43d70672da90
출처 데이터셋
uspto-grants-2013_04
특허 번호
US08420646B2

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