Methanol → Methyl 4-methyl-3-nitrobenzoate

HRID 435142

反応式

HRID 435142 の反応式
[CH3:1][C:2]1[CH:10]=[CH:9][C:5]([C:6]([OH:8])=[O:7])=[CH:4][C:3]=1[N+:11]([O-:13])=[O:12].[CH3:14]O.S(=O)(=O)(O)O>O>[CH3:14][O:7][C:6]([C:5]1[CH:9]=[CH:10][C:2]([CH3:1])=[C:3]([N+:11]([O-:13])=[O:12])[CH:4]=1)=[O:8]

参加物

5

反応物 3

HCID 887MethanolHCID 1118Sulfuric AcidHCID 73194-Methyl-3-nitrobenzoic acid

生成物 1

HCID 81816Methyl 4-methyl-3-nitrobenzoate

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

Approximately 18.1 g of 4-methyl-3-nitrobenzoic acid was added to approximately 50 ml of methanol. Approximately 2 ml of concentrated sulfuric acid was added to this solution. The resulting solution was heated to reflux temperature and stirred at this temperature for 16 hours. The solution was cooled and approximately 300 ml of water was added. The resulting composition was extracted with 200 ml of ether. The ether phase was saved and the aqueous phase was discarded. The ether phase was then sequentially washed with 100 ml of water, followed by 100 ml of 10% aqueous sodium carbonate. The ether phase was dried over magnesium sulfate, filtered, and concentrated using a rotary evaporator and a water aspirator vacuum to yield 17.3 g of 4-methoxycarbonyl-2-nitrotoluene as a viscous oil.

後処理

  1. temperatureThe resulting solution was heated
  2. temperatureto reflux temperature
  3. temperatureThe solution was cooled
  4. extractionThe resulting composition was extracted with 200 ml of ether
  5. washThe ether phase was then sequentially washed with 100 ml of water
  6. dry with materialThe ether phase was dried over magnesium sulfate
  7. filtrationfiltered
  8. concentrationconcentrated
  9. customa rotary evaporator

出典と根拠

ORDレコード
ord-cb758bfd24dc44a2888cc0a9287c694b
出典データセット
uspto-grants-1983_08
特許番号
US04400461

関連ノート

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