Formamide → HCID 22648863、化合物

HRID 393287ノート

反応式

HRID 393287 の反応式
Br[CH2:2][C:3]([C:5]1[CH:10]=[CH:9][C:8]([OH:11])=[C:7]([CH3:12])[CH:6]=1)=O.[CH:13]([NH2:15])=[O:14]>>[O:14]1[CH:2]=[C:3]([C:5]2[CH:10]=[CH:9][C:8]([OH:11])=[C:7]([CH3:12])[CH:6]=2)[N:15]=[CH:13]1

参加物

3

反応物 2

HCID 713FormamideHCID 112184492-Bromo-1-(4-hydroxy-3-methylphenyl)ethanone

生成物 1

HCID 22648863HCID 22648863、化合物収率 33%

実験手順

A solution of 2-bromo-1-(4-hydroxy-3-methylphenyl)ethanone (200 mg, 0.87 mmol) in formamide (10 mL) was heated to 110° C. for 24 h. The excess formamide was removed by distillation under reduced pressure. The resulting residue was partitioned between a pH 7.0 buffer solution (10 mL) and EtOAc (50 mL). The organic layer was washed with water (10 mL) and brine (10 mL), dried (MgSO4), filtered and concentrated under reduced pressure. The residue was purified by flash chromatography (Hexane:EtOAc, 1:1) to yield the title compound (51 mg, 33% yield).

後処理

  1. customThe excess formamide was removed by distillation under reduced pressure
  2. customThe resulting residue was partitioned between a pH 7.0 buffer solution (10 mL) and EtOAc (50 mL)
  3. washThe organic layer was washed with water (10 mL) and brine (10 mL)
  4. dry with materialdried (MgSO4)
  5. filtrationfiltered
  6. concentrationconcentrated under reduced pressure
  7. customThe residue was purified by flash chromatography (Hexane:EtOAc, 1:1)

出典と根拠

ORDレコード
ord-f61df3abbbf64cc7a48e7f723b7b5a9d
出典データセット
uspto-grants-2004_10
特許番号
US06806265B2

反応ノート

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