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Sodium Hydroxide → 2-Oxo-1,2,3,4-tetrahydroquinoline-6-carboxylic acid

HRID 358483
ノート
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反応式

HRID 358483 の反応式
[OH-:1].[Na+].BrC(Br)[C:5]([C:7]1[CH:8]=[C:9]2[C:14](=[CH:15][CH:16]=1)[NH:13][C:12](=[O:17])[CH2:11][CH2:10]2)=[O:6]>O>[C:5]([C:7]1[CH:8]=[C:9]2[C:14](=[CH:15][CH:16]=1)[NH:13][C:12](=[O:17])[CH2:11][CH2:10]2)([OH:6])=[O:1]
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 14798Sodium HydroxideHCID 131049236-(Dibromoacetyl)-3,4-dihydroquinolin-2(1H)-one

生成物 1

HCID 71319092-Oxo-1,2,3,4-tetrahydroquinoline-6-carboxylic acid収率 54.5%

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

Into 250 ml of water, 26 g sodium hydroxide was dissolved, then at a temperature of 90°-100° C. and under stirring condition, 35 g of 6-dibromoacetyl-3,4-dihydrocarbostyril was added thereinto and reacted for 3 hours. After the reaction was completed, the reaction mixture was cooled and insoluble matters formed in the mixture were removed by filtration. The mother liquor was acidified with concentrated hydrochloric acid and the crystals precipitated were collected by filtration and washed with water. The crystals thus obtained were recrystallized from ethanol twice to obtain 10.5 g of 6-carboxy-3,4-dihydrocarbostyril in the form of light yellow amorphous crystals. Melting point: 324.5°-327° C. (decomposed).

後処理

  1. additionwas added
  2. customreacted for 3 hours
  3. temperaturethe reaction mixture was cooled
  4. custominsoluble matters formed in the mixture
  5. customwere removed by filtration
  6. customthe crystals precipitated
  7. filtrationwere collected by filtration
  8. washwashed with water
  9. customThe crystals thus obtained
  10. customwere recrystallized from ethanol twice

出典と根拠

ORDレコード
ord-d71d599c67f74ca480f68de0ffe9a68a
出典データセット
uspto-grants-1984_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04468402

反応ノート

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