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

HRID 518826ノート

反応式

HRID 518826 の反応式
[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

参加物

5

反応物 3

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

生成物 1

HCID 866979922-Chloro-4-isopropoxy-5-nitropyridine収率 61%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-6ce76442920749218b7376c694ac50e3
出典データセット
uspto-grants-2015_08
特許番号
US09115140B2

反応ノート

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