Hydrochloric Acid → HCID 178418525、化合物

HRID 4795

反応式

HRID 4795 の反応式
[OH:1][C:2]1[N:10]=[CH:9][CH:8]=[CH:7][C:3]=1[C:4]([OH:6])=[O:5].[OH-].[Na+].[Br:13][O-].[Na+].BrBr.Cl>O>[Br:13][C:8]1[CH:7]=[C:3]([C:4]([OH:6])=[O:5])[C:2]([OH:1])=[N:10][CH:9]=1

参加物

7

反応物 5

HCID 313Hydrochloric AcidHCID 14798Sodium Hydroxide2 回HCID 24408BromineHCID 23673712Sodium hypobromite2 回HCID 178418543HCID 178418543、化合物

生成物 1

HCID 178418525HCID 178418525、化合物収率 63.5%

試薬・触媒・溶媒 1

HCID 962Water溶媒2 回

実験手順

To a solution of 10 g (0.07 mole) of 2-hydroxy-nicotinic acid in 16.8 g of 50% sodium hydroxide (0.21 mole) diluted with 25 ml of water was added 200 ml of sodium hypobromite solution prepared by adding 13.6 g (0.17 mole) of bromine to a solution of 20.16 g of 50% sodium hydroxide (0.25 mole) in 125 ml of water at 0° C. diluted to 400 ml. After 24 hrs of stirring at room temperature, another 100 ml portion of the above sodium hypobromite solution was added and the reaction solution was stirred for another 24 hr. The reaction solution was cooled in an ice bath and acidified carefully with 12N hydrochloric acid. Crystallization from isopropyl alcohol gave 9.7 g (63.5%) of product. A sample was further recrystallized from 95% ethanol, m.p. 245° C.

後処理

  1. customprepared
  2. additiondiluted to 400 ml
  3. stirringthe reaction solution was stirred for another 24 hr
  4. temperatureThe reaction solution was cooled in an ice bath
  5. customCrystallization from isopropyl alcohol

出典と根拠

ORDレコード
ord-f3db1044f1d24b8cbe93aa3f0f632b1b
出典データセット
uspto-grants-1988_02
特許番号
US04727152

関連ノート

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