Hydrochloric Acid → HCID 178418525, 화합물

HRID 247263

반응식

HRID 247263 반응식
[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

참가 물질

7

반응물 5

HCID 313Hydrochloric AcidHCID 14798Sodium Hydroxide2회HCID 24408BromineHCID 23673712Sodium hypobromite2회HCID 178418543HCID 178418543, 화합물

생성물 1

HCID 178418525HCID 178418525, 화합물수율 63.5%

시약·촉매·용매 1

HCID 962Water용매2회

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-8cfd15f6bdde4a7db063bcbf10d2d4a9
출처 데이터셋
uspto-grants-1987_11
특허 번호
US04705853

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