Potassium Carbonate → HCID 18455594、化合物

HRID 1820642ノート

反応式

HRID 1820642 の反応式
[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

参加物

6

反応物 4

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

生成物 1

HCID 18455594HCID 18455594、化合物収率 63.6%

試薬・触媒・溶媒 1

HCID 6342Acetonitrile溶媒

実験手順

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.

後処理

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

出典と根拠

ORDレコード
ord-ae9b1dda40d64534a0b56ebd1e2e50ef
出典データセット
uspto-grants-2009_10
特許番号
US07605157B2

反応ノート

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