Hydrochloric Acid → 4-Acetamidosalicylic acid

HRID 2107017

反応式

HRID 2107017 の反応式
[OH:1][C:2]1[CH:10]=[C:9]([NH2:11])[CH:8]=[CH:7][C:3]=1[C:4]([O-:6])=[O:5].[Na+].Cl.[C:14](OC(=O)C)(=[O:16])[CH3:15]>O>[OH:1][C:2]1[CH:10]=[C:9]([NH:11][C:14](=[O:16])[CH3:15])[CH:8]=[CH:7][C:3]=1[C:4]([OH:6])=[O:5]

参加物

5

反応物 3

HCID 313Hydrochloric AcidHCID 7918Acetic AnhydrideHCID 2724368Aminosalicylate sodium anhydrous

生成物 1

HCID 655094-Acetamidosalicylic acid収率 56%

試薬・触媒・溶媒 1

HCID 962Water溶媒2 回

反応条件

温度
100 °C

実験手順

Sodium 2-hydroxy-4-aminobenzoate (76 g, 0.437 mole) was dissolved in water (2-300 ml) and concentrated hydrochloric acid (36.2 ml) was added after which the precipitated crystalline free acid was isolated by filtration. The acid was suspended in water (700 ml), acetic anhydride (48 ml) was added and the mixture was heated to about 100° C. (supplied with a reflux condenser) for 15 minutes under nitrogen. After cooling, the crystalline material was filtered off and dried in vacuo to give the title compound (48 g, 56%), m.p. 221°-223° C. Found (Calc. for C9H9NO4) C 55.14 (55.38), H 4.73 (4.62), N 7.12 (7.18).

後処理

  1. customwas isolated by filtration
  2. temperatureAfter cooling
  3. filtrationthe crystalline material was filtered off
  4. customdried in vacuo

出典と根拠

ORDレコード
ord-b629cd53f4a44aa783759b3f39a6ea85
出典データセット
uspto-grants-1990_06
特許番号
US04933330

関連ノート

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