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Sulfuric Acid → 5-Acetyl-6-methyl-2-oxo-1,2-dihydropyridine-3-carboxylic acid

HRID 637958
ノート
印刷プレビュー

反応式

HRID 637958 の反応式
[C:1]([C:4]1[CH:12]=[C:8]([C:9](N)=[O:10])[C:7](=[O:13])[NH:6][C:5]=1[CH3:14])(=[O:3])[CH3:2].S(=O)(=O)(O)[OH:16]>O>[C:1]([C:4]1[CH:12]=[C:8]([C:9]([OH:16])=[O:10])[C:7](=[O:13])[NH:6][C:5]=1[CH3:14])(=[O:3])[CH3:2]
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 1118Sulfuric AcidHCID 27644175-Acetyl-6-methyl-2-oxo-1,2-dihydropyridine-3-carboxamide

生成物 1

HCID 132320405-Acetyl-6-methyl-2-oxo-1,2-dihydropyridine-3-carboxylic acid

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

A mixture containing 34 g of 5-acetyl-1,2-dihydro-6-methyl-2-oxonicotinamide, 50 ml of concentrated sulfuric acid and 100 ml of water was heated on a steam bath with stirring for 6 hours. The hot reaction solution was filtered and to the filtrate was added 50 ml of water. The resulting mixture was allowed to stand at room temperature overnight whereupon the product crystallized out. The separated product was collected, washed with water, dried in a vacuum oven at 90°-95° C. to yield 16.8 g of 5-acetyl-1,2-dihydro-6-methyl-2-oxonicotinic acid, m.p. 238°-241° C. This acid was recrystallized from methanol and dried to yield 14.7 g of 5-acetyl-1,2-dihydro-6-methyl-2-oxonicotinic acid, m.p. 241°-243° C.

後処理

  1. temperaturewas heated on a steam bath
  2. filtrationThe hot reaction solution was filtered and to the filtrate
  3. additionwas added 50 ml of water
  4. waitto stand at room temperature overnight whereupon the product
  5. customcrystallized out
  6. customThe separated product was collected
  7. washwashed with water
  8. customdried in a vacuum oven at 90°-95° C.

出典と根拠

ORDレコード
ord-08b661d5643b4b5cae360e1cfde66ba1
出典データセット
uspto-grants-1985_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04559347

反応ノート

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