Sodium Hydroxide → 1-Amino-1,4-dihydro-7-methyl-4-oxo-1,8naphthyridine-3-carboxylic acid

HRID 462693ノート

反応式

HRID 462693 の反応式
[NH2:1][N:2]1[C:11]2[C:6](=[CH:7][CH:8]=[C:9]([CH3:12])[N:10]=2)[C:5](=[O:13])[C:4]([C:14]([O:16]CC)=[O:15])=[CH:3]1.[OH-].[Na+]>O>[NH2:1][N:2]1[C:11]2[C:6](=[CH:7][CH:8]=[C:9]([CH3:12])[N:10]=2)[C:5](=[O:13])[C:4]([C:14]([OH:16])=[O:15])=[CH:3]1

参加物

4

反応物 2

HCID 14798Sodium HydroxideHCID 13457701Ethyl 1-amino-1,4-dihydro-7-methyl-4-oxo-1,8-naphthyridine-3-carboxylate

生成物 1

HCID 134577021-Amino-1,4-dihydro-7-methyl-4-oxo-1,8naphthyridine-3-carboxylic acid収率 88%

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

A mixture of 10.0 g (0.0405 m) of ethyl 1-amino-1,4-dihydro-7-methyl-4-oxo-1,8-naphthyridine-3-carboxylate, 1.94 g (0.0486 m) of sodium hydroxide and 350 ml of water was heated on a steam bath for two hours. The resulting solution was filtered, cooled and neutralized with 3 ml of acetic acid while stirring. The solid product was collected by filtration, washed with water and recrystallized by dissolving it in 100 ml of boiling dimethylformamide and adding 100 ml of ether to the cooled solution. There was obtained 7.8 g of 1-amino-1,4-dihydro-7-methyl-4-oxo-1,8naphthyridine-3-carboxylic acid, colorless needles, m.p. 239°-240° C.

後処理

  1. temperaturewas heated on a steam bath for two hours
  2. filtrationThe resulting solution was filtered
  3. temperaturecooled
  4. filtrationThe solid product was collected by filtration
  5. washwashed with water
  6. customrecrystallized
  7. dissolutionby dissolving it in 100 ml of boiling dimethylformamide
  8. additionadding 100 ml of ether to the cooled solution

出典と根拠

ORDレコード
ord-f17a047c05be434e964e15839c0edb8a
出典データセット
uspto-grants-1985_05
特許番号
US04517191

反応ノート

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