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

HRID 637958
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HRID 637958 반응식
[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]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

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

생성물 1

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

시약·촉매·용매 1

HCID 962Water용매

실험 절차

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.

후처리

  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.

출처 및 근거

ORD 기록
ord-08b661d5643b4b5cae360e1cfde66ba1
출처 데이터셋
uspto-grants-1985_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04559347

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