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

HRID 661102ノート

反応式

HRID 661102 の反応式
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

参加物

6

反応物 5

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

生成物 1

HCID 226029855-Bromo-2-iodopyridin-3-ol収率 99.4%

実験手順

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).

後処理

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

出典と根拠

ORDレコード
ord-1a5407e86b4140a59bfae67480841bd8
出典データセット
uspto-grants-2011_12
特許番号
US08084479B2

反応ノート

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