Water → HCID 66757224, 화합물

HRID 1642597노트

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HRID 1642597 반응식
[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

참가 물질

6

반응물 4

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

생성물 1

HCID 66757224HCID 66757224, 화합물

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

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온도
65 °C

실험 절차

To a solution of 5-iodo-2-nitrophenol (2.65 g, 10 mmol) [J Org Chem, Vol. 63, pp. 4199-4208 (1998)] 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.

후처리

  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

출처 및 근거

ORD 기록
ord-045a1fbbe8c146b8a551b1fc5ce5b54d
출처 데이터셋
uspto-grants-2012_02
특허 번호
US08119666B2

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