Bromine → HCID 178508959、化合物

HRID 1848361ノート

反応式

HRID 1848361 の反応式
[NH2:1][C:2]1[CH:7]=[CH:6][CH:5]=[C:4]([OH:8])[N:3]=1.[Br:9]Br>C(O)(=O)C>[NH2:1][C:2]1[N:3]=[C:4]([OH:8])[CH:5]=[CH:6][C:7]=1[Br:9]

参加物

4

反応物 2

HCID 24408BromineHCID 1785076342-Amino-6-hydroxypyridine

生成物 1

HCID 178508959HCID 178508959、化合物収率 68.4%

試薬・触媒・溶媒 1

HCID 176Acetic Acid溶媒

実験手順

Under an argon atmosphere 2-amino-6-hydroxy-pyridine (19.6 g, 178 mmol) was suspended in acetic acid (100%, 390 mL). Br2 (9.2 mL, 178 mmol) was added at 20° C. over 5 min. The green suspension was stirred at RT for 20 min. The mixture was poured onto H2O (400 mL) and filtered. The filtrate was mixed with brine (200 mL) and extracted with EtOAc (10×400 mL). The combined organic phases were dried (Na2SO4), filtered and concentrated to afford 6-Amino-5-bromo-pyridin-2-ol as a yellow solid (23 g).

後処理

  1. additionThe mixture was poured onto H2O (400 mL)
  2. filtrationfiltered
  3. additionThe filtrate was mixed with brine (200 mL)
  4. extractionextracted with EtOAc (10×400 mL)
  5. dry with materialThe combined organic phases were dried (Na2SO4)
  6. filtrationfiltered
  7. concentrationconcentrated

出典と根拠

ORDレコード
ord-67d97185f367497a8a7718dd8ad8a328
出典データセット
uspto-grants-2015_02
特許番号
US08952162B2

反応ノート

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