Water → HCID 66757224、化合物

HRID 660472ノート

反応式

HRID 660472 の反応式
[I:1][C:2]1[CH:3]=[CH:4][C:5]([N+:9]([O-:11])=[O:10])=[C:6]([OH:8])[CH:7]=1.[CH2:12](Br)[C:13]1[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=1.C([O-])([O-])=O.[K+].[K+].O>CN(C=O)C>[CH2:12]([O:8][C:6]1[CH:7]=[C:2]([I:1])[CH:3]=[CH:4][C:5]=1[N+:9]([O-:11])=[O:10])[C:13]1[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=1

参加物

6

反応物 4

HCID 962WaterHCID 7498Benzyl BromideHCID 11430Potassium CarbonateHCID 140916895-Iodo-2-nitrophenol

生成物 1

HCID 66757224HCID 66757224、化合物

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

反応条件

温度
65 °C

実験手順

To a solution of 5-iodo-2-nitrophenol (2.65 g, 10 mmol) (J. Org. Chem. 1998, 63, 4199-4208) in DMF (10 mL) is added benzyl bromide (1.71 g, 10 mmol) and K2CO3 (2.07 g, 15 mmol) and the mixture is heated at 65° C. for 30 min. Then water is added (400 mL) and it is extracted by EtOAc (2×200 mL). The water layer is then acidified and extracted with EtOAc (100 mL). The combined EtOAc layer is then washed with 1N HCl and brine, dried with NaSO4 and concentrated to give the title compound as a yellow solid.

後処理

  1. extractionis extracted by EtOAc (2×200 mL)
  2. extractionextracted with EtOAc (100 mL)
  3. washThe combined EtOAc layer is then washed with 1N HCl and brine
  4. dry with materialdried with NaSO4
  5. concentrationconcentrated

出典と根拠

ORDレコード
ord-c029fab11a594a5e8f615d0d05f3c7ce
出典データセット
uspto-grants-2011_12
特許番号
US08084448B2

反応ノート

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