Methanol → Methyl 2-iodo-5-nitrobenzoate

HRID 381290

反応式

HRID 381290 の反応式
[I:1][C:2]1[CH:10]=[CH:9][C:8]([N+:11]([O-:13])=[O:12])=[CH:7][C:3]=1[C:4]([OH:6])=[O:5].S(=O)(=O)(O)O.[CH3:19]O>>[I:1][C:2]1[CH:10]=[CH:9][C:8]([N+:11]([O-:13])=[O:12])=[CH:7][C:3]=1[C:4]([O:6][CH3:19])=[O:5]

参加物

4

反応物 3

HCID 887MethanolHCID 1118Sulfuric AcidHCID 38487452-Iodo-5-nitrobenzoic acid

生成物 1

HCID 11415548Methyl 2-iodo-5-nitrobenzoate

実験手順

In a 5 liter 3 necked flask, 2-iodo-5-nitro-benzoic acid (100 grams) was dissolved in methanol (3000 ml). The flask was fitted with a reflux condenser and 50 ml of concentrated sulfuric acid was added carefully with cooling. After the completion of the addition, the contents were refluxed for 3 days until completion of the reaction. The reaction was followed by TLC. After the completion of the reaction, the reaction mixture was concentrated to 1000 ml and allowed to cool. The product crystalized as a light yellow colored powder. The solid material was filtered and washed with water and methanol and air-dried. The yield was 90 grams.

後処理

  1. customThe flask was fitted with a reflux condenser
  2. temperaturewith cooling
  3. additionAfter the completion of the addition
  4. temperaturethe contents were refluxed for 3 days until completion of the reaction
  5. customAfter the completion of the reaction
  6. concentrationthe reaction mixture was concentrated to 1000 ml
  7. temperatureto cool
  8. customThe product crystalized as a light yellow colored powder
  9. filtrationThe solid material was filtered
  10. washwashed with water and methanol
  11. customair-dried

出典と根拠

ORDレコード
ord-5ff507e7e7ad407ca2023eeafe0ea16d
出典データセット
uspto-grants-2001_10
特許番号
US06306871B1

関連ノート

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