Methanol → Methyl 2-(2-chlorobenzylideneaminooxymethyl)-2-methylpropanoate

HRID 1722517ノート

反応式

HRID 1722517 の反応式
[Cl:1][C:2]1[CH:17]=[CH:16][CH:15]=[CH:14][C:3]=1[CH:4]=[N:5][O:6][CH2:7][C:8]([CH3:13])([CH3:12])[C:9]([OH:11])=[O:10].S(=O)(=O)(O)O.[CH3:23]O>>[Cl:1][C:2]1[CH:17]=[CH:16][CH:15]=[CH:14][C:3]=1[CH:4]=[N:5][O:6][CH2:7][C:8]([CH3:13])([CH3:12])[C:9]([O:11][CH3:23])=[O:10]

参加物

4

反応物 3

HCID 887MethanolHCID 1118Sulfuric AcidHCID 542687412-(2-Chlorobenzylideneaminooxymethyl)-2-methylpropanoic acid

生成物 1

HCID 54572932Methyl 2-(2-chlorobenzylideneaminooxymethyl)-2-methylpropanoate

実験手順

A solution of 2-(2-chlorobenzylideneaminooxymethyl)-2-methylpropanoic acid (31.6 grams; 0.12 mole) and concentrated sulfuric acid (2 mL) in methanol (100 mL) was heated at reflux for two hours and then stirred for 48 hours at ambient temperature. The reaction mixture was then heated for an additional four hours. The reaction mixture was concentrated under reduced pressure. Water (30 mL) and methylene chloride (30 mL) were added to the residue. The mixture was then neutralized with aqueous sodium carbonate and extracted with methylene chloride. The dried (magnesium sulfate) extract was concentrated under reduced pressure to yield 27.0 grams of methyl 2-(2-chlorobenzylideneaminooxymethyl)-2-methylpropanoate.

後処理

  1. temperatureat reflux for two hours
  2. temperatureThe reaction mixture was then heated for an additional four hours
  3. concentrationThe reaction mixture was concentrated under reduced pressure
  4. additionWater (30 mL) and methylene chloride (30 mL) were added to the residue
  5. extractionextracted with methylene chloride
  6. dry with materialThe dried (magnesium sulfate)
  7. extractionextract
  8. concentrationwas concentrated under reduced pressure

出典と根拠

ORDレコード
ord-93d426f8d74141a5ba796f1a38bb62ea
出典データセット
uspto-grants-1989_08
特許番号
US04855480

反応ノート

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