Water → 2,6-Diiodo-3-methoxy-4-(3-methoxy-propoxy)pyridine

HRID 2263549노트

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HRID 2263549 반응식
[OH-].[Na+].[I:3][C:4]1[C:9]([O:10][CH3:11])=[C:8]([OH:12])[CH:7]=[C:6]([I:13])[N:5]=1.I[CH2:15][CH2:16][CH2:17][O:18][CH3:19].O>CN(C)C=O.C(OCC)(=O)C>[I:3][C:4]1[C:9]([O:10][CH3:11])=[C:8]([O:12][CH2:15][CH2:16][CH2:17][O:18][CH3:19])[CH:7]=[C:6]([I:13])[N:5]=1

참가 물질

7

반응물 4

HCID 962WaterHCID 14798Sodium HydroxideHCID 135229891-Iodo-3-methoxypropaneHCID 178493893HCID 178493893, 화합물

생성물 1

HCID 231494742,6-Diiodo-3-methoxy-4-(3-methoxy-propoxy)pyridine

시약·촉매·용매 2

HCID 6228Dimethylformamide용매HCID 8857Ethyl Acetate용매

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온도
0 °C

실험 절차

To a stirred solution of 60 mmol NaOH in 50 ml N,N-dimethyl formamide is progressively added 50 mmol 2,6-diiodo-3-methoxy-pyridin-4-ol [437709-87-0]. The reaction mixture is stirred for 30 minutes and then cooled to 0° C. 60 mmol 1-iodo-3-methoxy-propane [61542-10-7] are added and the mixture is stirred for 15 minutes at room temperature. Water and ethyl acetate are added to the mixture, the layers are separated and the aqueous layer is extracted with ethyl acetate (3×). The combined organic layers are dried over sodium sulphate, filtered and concentrated. The title compound is obtained from the residue by means of flash chromatography (SiO2 60 F) and identified based on its Rf value,

후처리

  1. stirringthe mixture is stirred for 15 minutes at room temperature
  2. customthe layers are separated
  3. extractionthe aqueous layer is extracted with ethyl acetate (3×)
  4. dry with materialThe combined organic layers are dried over sodium sulphate
  5. filtrationfiltered
  6. concentrationconcentrated

출처 및 근거

ORD 기록
ord-62972de1f87a42c7bb8d96c835e973f9
출처 데이터셋
uspto-grants-2010_12
특허 번호
US07851634B2

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