Water → 2-Chloro-4-isopropoxy-5-nitropyridine

HRID 518826노트

반응식

HRID 518826 반응식
[CH3:1][CH:2]([CH3:4])[O-:3].[Na+].[Cl:6][C:7]1[CH:12]=[C:11](Cl)[C:10]([N+:14]([O-:16])=[O:15])=[CH:9][N:8]=1.O>CN(C=O)C>[Cl:6][C:7]1[CH:12]=[C:11]([O:3][CH:2]([CH3:4])[CH3:1])[C:10]([N+:14]([O-:16])=[O:15])=[CH:9][N:8]=1

참가 물질

5

반응물 3

HCID 962WaterHCID 109204432-Propanol, sodium salt (1:1)2회HCID 122757652,4-Dichloro-5-nitropyridine

생성물 1

HCID 866979922-Chloro-4-isopropoxy-5-nitropyridine수율 61%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

3.38 g of sodium isopropoxide are added to a solution of 2.6 g of 2.4-dichloro-5-nitropyridine in 39 ml of DMF. The reaction medium is stirred at ambient temperature for 1 h 15 and 3.18 g of sodium isopropoxide are added. The reaction medium is stirred for a further 15 minutes and then the mixture is poured into 200 ml of water and extracted with ethyl acetate. The organic phase is dried over magnesium sulfate, filtered and concentrated under reduced pressure. Purification is carried out by flash chromatography on silica gel (40-63 microns), elution being carried out with a heptane/ethyl acetate mixture (90/10 to 80/20). 1.78 g of 2-chloro-5-nitro-4-(propan-2-yloxy)pyridine are obtained in the form of a pale yellow solid.

후처리

  1. additionare added
  2. extractionextracted with ethyl acetate
  3. dry with materialThe organic phase is dried over magnesium sulfate
  4. filtrationfiltered
  5. concentrationconcentrated under reduced pressure
  6. customPurification
  7. washis carried out by flash chromatography on silica gel (40-63 microns), elution

출처 및 근거

ORD 기록
ord-6ce76442920749218b7376c694ac50e3
출처 데이터셋
uspto-grants-2015_08
특허 번호
US09115140B2

반응 노트

불러오는 중…