Hydrochloric Acid → 6-Bromo-1H-indazole-3-carboxylic acid

HRID 407152

반응식

HRID 407152 반응식
[Br:1][C:2]1[CH:10]=[C:9]2[C:5]([C:6](=O)[C:7](=O)[NH:8]2)=[CH:4][CH:3]=1.[N:13]([O-])=O.[Na+].S(=O)(=O)(O)O.Cl.[OH2:23].[OH2:24].Cl[Sn]Cl>[OH-].[Na+].O>[Br:1][C:2]1[CH:10]=[C:9]2[C:5]([C:6]([C:7]([OH:24])=[O:23])=[N:13][NH:8]2)=[CH:4][CH:3]=1

참가 물질

8

반응물 5

HCID 313Hydrochloric AcidHCID 1118Sulfuric AcidHCID 61436Stannous chloride dihydrateHCID 957161H-Indole-2,3-dione, 6-bromo-HCID 23668193Sodium Nitrite

생성물 1

HCID 247280286-Bromo-1H-indazole-3-carboxylic acid수율 169.3%

시약·촉매·용매 2

HCID 962Water용매2회HCID 14798Sodium Hydroxide용매

반응 조건

온도
0 °C

실험 절차

The solution of 6-bromoisatin (10 g, 22 mmol) in 1N aqueous NaOH solution (48 Ml) was stirred at 50° C. for 1 h. The mixture was cooled to 0° C. Sodium nitrite (3 g, 22 mmol) solution in water (11 Ml) was added dropwise for 15 min at 0° C. The mixture was added to the solution of water (90 Ml) and sulfuric acid (4.6 Ml) at 0° C. for 15 min. The mixture was added to the solution of conc. hydrochloric acid (40 Ml) and SnCl2.2H2O (24 g, 53 mmol). After 1 h, the mixture was filtered and washed with water. The solid was dried through air flow to give the titled compound (8.98 g).

후처리

  1. filtrationthe mixture was filtered
  2. washwashed with water
  3. customThe solid was dried through air flow

출처 및 근거

ORD 기록
ord-ea057a89e8594ee181d07db68154d2d4
출처 데이터셋
uspto-grants-2014_06
특허 번호
US08754209B2

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