Sodium Iodide → HCID 18938755, 화합물

HRID 356579노트

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HRID 356579 반응식
[CH3:1][O:2][CH:3]([O:14][CH3:15])[C:4]1[CH:9]=[C:8]([OH:10])[CH:7]=[CH:6][C:5]=1[N+:11]([O-:13])=[O:12].C(=O)([O-])[O-].[K+].[K+].[I-].[Na+].Cl[CH2:25][CH2:26][CH2:27][OH:28]>CN(C=O)C.C(OCC)(=O)C>[CH3:15][O:14][CH:3]([O:2][CH3:1])[C:4]1[CH:9]=[C:8]([O:10][CH2:25][CH2:26][CH2:27][OH:28])[CH:7]=[CH:6][C:5]=1[N+:11]([O-:13])=[O:12]

참가 물질

7

반응물 4

HCID 5238Sodium IodideHCID 11430Potassium CarbonateHCID 123133-Chloro-1-propanolHCID 32847943-(Dimethoxymethyl)-4-nitrophenol

생성물 1

HCID 18938755HCID 18938755, 화합물수율 94.2%

시약·촉매·용매 2

HCID 6228Dimethylformamide용매HCID 8857Ethyl Acetate용매

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온도
70 °C

실험 절차

5-Hydroxy-2-nitrobenzaldehyde dimethyl acetal (5.33 g) is dissolved in dry DMF (50 ml), and thereto are added potassium carbonate (6.91 g), sodium iodide (7.5 g) and 3-chloropropanol (4.73 g), and the mixture is stirred at 70° C. for 22 hours. To the mixture is added ethyl acetate, and the insoluble materials are removed by filtration. The filtrate is concentrated under reduced pressure, and the residue is purified by silica gel column chromatography to give 5-(3'-hydroxypropyloxy)-2-nitrobenzaldehyde dimethyl acetal (6.39 g) as a pale yellow oil.

후처리

  1. customthe insoluble materials are removed by filtration
  2. concentrationThe filtrate is concentrated under reduced pressure
  3. customthe residue is purified by silica gel column chromatography

출처 및 근거

ORD 기록
ord-bb242bafddaf46b0b4bcd1556637bb8a
출처 데이터셋
uspto-grants-1998_11
특허 번호
US05837673

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