Hydrochloric Acid → 5-Bromo-2-iodopyridin-3-ol

HRID 661102노트

반응식

HRID 661102 반응식
O.C(=O)([O-])[O-].[Na+].[Na+].[Br:8][C:9]1[CH:10]=[N:11][CH:12]=[C:13]([OH:15])[CH:14]=1.O.[I:17]I.Cl>>[Br:8][C:9]1[CH:14]=[C:13]([OH:15])[C:12]([I:17])=[N:11][CH:10]=1

참가 물질

6

반응물 5

HCID 313Hydrochloric AcidHCID 807IodineHCID 962WaterHCID 5995293-Bromo-5-hydroxypyridineHCID 2735133Sodium Carbonate Monohydrate

생성물 1

HCID 226029855-Bromo-2-iodopyridin-3-ol수율 99.4%

실험 절차

To a mixture of sodium carbonate monohydrate (1.96 mL, 35.5 mmol) and 3-bromo-5-hydroxypyridine (2.06 g, 11.8 mmol) in H2O (0.213 mL, 11.8 mmol) was added iodine crystals (0.640 mL, 12.4 mmol), and the overall mixture was stirred at room temperature overnight. The mixture was then poured slowly into 2M HCl(aq), and the pH was adjusted to ˜3. The product was collected by filtration followed by crystallization from EtOH/water to afford 5-bromo-2-iodopyridin-3-ol as an off-white solid of (3.53 g, 99.4% yield) m/z (%): 301.2 (100%, M++H).

후처리

  1. filtrationThe product was collected by filtration
  2. customfollowed by crystallization from EtOH/water

출처 및 근거

ORD 기록
ord-1a5407e86b4140a59bfae67480841bd8
출처 데이터셋
uspto-grants-2011_12
특허 번호
US08084479B2

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