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Methanol → HCID 57743038, 화합물

HRID 1896457
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HRID 1896457 반응식
[Br:1][C:2]1[C:3]([C:11]([OH:13])=[O:12])=[C:4]2[NH:10][CH:9]=[N:8][C:5]2=[N:6][CH:7]=1.OS(O)(=O)=O.[CH3:19]O>>[Br:1][C:2]1[C:3]([C:11]([O:13][CH3:19])=[O:12])=[C:4]2[NH:10][CH:9]=[N:8][C:5]2=[N:6][CH:7]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 3

HCID 887MethanolHCID 1118Sulfuric AcidHCID 20501306-Bromo-3H-imidazo[4,5-B]pyridine-7-carboxylic acid

생성물 1

HCID 57743038HCID 57743038, 화합물수율 70%

실험 절차

Absolute methanol (30 ml) is added to 6-bromo-1H-imidazo[4,5-b]pyridine-7-carboxylic acid x208 (Zerenex; 2.2 g, 9.1 mmol). Concentrated H2SO4 (4 ml) is added to the obtained suspension at 0° C. The reaction mixture is refluxed under protection from the air moisture and vigorous stirring for 10 h. The reaction mixture is then evaporated to half-volume in the vacuum of a rotary evaporator and neutralized under cooling with ice with aqueous ammonia to pH 8-9. The formed precipitate is quickly separated by filtration, washed with ice-cold water (2×30 ml), and dried over P2O5 at 1 mmHg overnight to afford methyl 6-bromo-1H-imidazo[4,5-b]pyridine-7-carboxylate x209 (1.63 g).

후처리

  1. temperatureThe reaction mixture is refluxed under protection from the air moisture
  2. customThe reaction mixture is then evaporated to half-volume in the vacuum of a rotary evaporator
  3. temperatureunder cooling with ice with aqueous ammonia to pH 8-9
  4. customThe formed precipitate is quickly separated by filtration
  5. washwashed with ice-cold water (2×30 ml)
  6. dry with materialdried over P2O5 at 1 mmHg overnight

출처 및 근거

ORD 기록
ord-a3f823792af7452e81abe5f9ba510325
출처 데이터셋
uspto-grants-2013_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08518943B2

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