Hydrochloric Acid → HCID 21477059、化合物

HRID 2293535ノート

反応式

HRID 2293535 の反応式
N[C:2]1[C:3]([O:14][CH3:15])=[CH:4][C:5]([O:12][CH3:13])=[C:6]([CH:11]=1)[C:7]([O:9][CH3:10])=[O:8].N([O-])=O.[Na+].[ClH:20]>O.CC(C)=O>[Cl:20][C:2]1[C:3]([O:14][CH3:15])=[CH:4][C:5]([O:12][CH3:13])=[C:6]([CH:11]=1)[C:7]([O:9][CH3:10])=[O:8]

参加物

6

反応物 3

HCID 313Hydrochloric AcidHCID 16638096Methyl 5-amino-2,4-dimethoxybenzoateHCID 23668193Sodium Nitrite

生成物 1

HCID 21477059HCID 21477059、化合物

試薬・触媒・溶媒 2

HCID 180Acetone溶媒HCID 962Water溶媒2 回

実験手順

A 0.65 g portion of methyl 5-amino-2,4-dimethoxybenzoate was dissolved in a mixture solvent of 1.5 ml of water and 10 ml of acetone, and 1.3 ml of concentrated hydrochloric acid was added thereto, followed by dropwise addition of 0.23 g of sodium nitrite dissolved in 1 ml of water under ice-cooling and subsequent stirring for a while. Next, 0.35 g of cuprous chloride was added and the mixture was warmed up to room temperature. After completion of the reaction, insoluble matter was filtered and the resulting residue was mixed with water, extracted with ethyl acetate and then washed with water and saturated brine. After drying over anhydrous sodium sulfate, the solvent was evaporated under a reduced pressure and the resulting residue was purified by silica gel column chromatography (chloroform:methanol=500:1-40:1) to give 0.56 g of methyl 5-chloro-2,4-dimethoxybenzoate.

後処理

  1. additionwas added
  2. temperaturecooling
  3. customAfter completion of the reaction, insoluble matter
  4. filtrationwas filtered
  5. additionthe resulting residue was mixed with water
  6. extractionextracted with ethyl acetate
  7. washwashed with water and saturated brine
  8. dry with materialAfter drying over anhydrous sodium sulfate
  9. customthe solvent was evaporated under a reduced pressure
  10. customthe resulting residue was purified by silica gel column chromatography (chloroform:methanol=500:1-40:1)

出典と根拠

ORDレコード
ord-34f624603428400f8ccbec79ccec8f0a
出典データセット
uspto-grants-1997_11
特許番号
US05686482

反応ノート

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