Hydrochloric Acid → 6-Chloro-2-iodo-3-hydroxypyridine

HRID 269584ノート

反応式

HRID 269584 の反応式
[Cl:1][C:2]1[N:7]=[CH:6][C:5]([OH:8])=[CH:4][CH:3]=1.C(=O)([O-])[O-].[Na+].[Na+].[I:15]I.Cl>O>[Cl:1][C:2]1[N:7]=[C:6]([I:15])[C:5]([OH:8])=[CH:4][CH:3]=1

参加物

6

反応物 4

HCID 313Hydrochloric AcidHCID 807IodineHCID 10340Sodium CarbonateHCID 8198212-Chloro-5-hydroxypyridine

生成物 1

HCID 234331586-Chloro-2-iodo-3-hydroxypyridine

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

6-Chloro-3-pyridinol (2.0 g, 15.44 mmol) was stirred in water (40 ml) containing sodium carbonate (3.43 g, 32.36 mmol) and iodine (3.92 g, 15.44 mmol) was added. The mixture was stirred at room temperature for 72 hours. The pH was adjusted to pH8 with 1M hydrochloric acid solution and the mixture extracted with ethyl acetate (×2). The combined organic extracts were washed with brine and dried (MgSO4). The aqueous layer was acidified to pH5 with 1M hydrochloric acid solution and extracted with ethyl acetate, which was washed with brine, dried (MgSO4) and the combined solutions evaporated to leave the title compound as a buff solid (3.70 g).

後処理

  1. additionwas added
  2. extractionthe mixture extracted with ethyl acetate (×2)
  3. washThe combined organic extracts were washed with brine
  4. dry with materialdried (MgSO4)
  5. extractionextracted with ethyl acetate, which
  6. washwas washed with brine
  7. dry with materialdried (MgSO4)
  8. customthe combined solutions evaporated

出典と根拠

ORDレコード
ord-fda67ea3df394f178adaaec59d622444
出典データセット
uspto-grants-2008_11
特許番号
US07446222B2

反応ノート

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