Hydrochloric Acid → HCID 178418525, 화합물

HRID 238484

반응식

HRID 238484 반응식
[Br:1][O-].[Na+].BrBr.[OH:6][C:7]1[N:15]=[CH:14][CH:13]=[CH:12][C:8]=1[C:9]([OH:11])=[O:10].Cl>[OH-].[Na+]>[Br:1][C:13]1[CH:14]=[N:15][C:7]([OH:6])=[C:8]([CH:12]=1)[C:9]([OH:11])=[O:10]

참가 물질

6

반응물 4

HCID 313Hydrochloric AcidHCID 24408Bromine2회HCID 23673712Sodium hypobromite3회HCID 178418543HCID 178418543, 화합물2회

생성물 1

HCID 178418525HCID 178418525, 화합물

시약·촉매·용매 1

HCID 14798Sodium Hydroxide용매2회

반응 조건

온도
0 °C

실험 절차

A solution of sodium hypobromide was made by adding Br2 (1.01 ml, 39.5 mmol, 1.1 eq) slowly over a period of 5 min to NaOH (5N, 40 ml) that was previously cooled to 0° C. in an ice bath. The solution was stirred for 10 min before adding 2-hydroxynicotinic acid (5.0 g, 35.9 mmol) and placed in a 50° C. oil bath and stirred. Concurrently, a second pot of sodium hypobromide solution was made by slowly adding Br2 (1.01 ml, 39.5 mmol, 1.1 eq) to a NaOH solution (5N, 40 ml) in an ice bath. The second pot of sodium hypobromide was added to the solution of 2-hydroxynicotinic acid after 24 h of heating then was stirred for an additional 24 h. The solution was cooled to RT, placed in an ice bath and acidified with concentrated HCl while stirring. The precipitate which formed was filtered, washed and dried to afford the desired compound as an off-white solid.

후처리

  1. customplaced in a 50° C.
  2. stirringstirred
  3. temperatureof heating
  4. stirringthen was stirred for an additional 24 h
  5. temperatureThe solution was cooled to RT
  6. customplaced in an ice bath
  7. stirringwhile stirring
  8. customThe precipitate which formed
  9. filtrationwas filtered
  10. washwashed
  11. customdried

출처 및 근거

ORD 기록
ord-79764d535c0b47359d2d5159489f4e7e
출처 데이터셋
uspto-grants-2014_02
특허 번호
US08642624B2

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