HCID 178470035、化合物 → HCID 178516647、化合物

HRID 386414

反応式

HRID 386414 の反応式
C(OC(=O)[C:5]1[C:10]([OH:11])=[CH:9][C:8]([C:12]([F:15])([F:14])[F:13])=[N:7][C:6]=1[OH:16])C>Cl>[F:15][C:12]([F:13])([F:14])[C:8]1[N:7]=[C:6]([OH:16])[CH:5]=[C:10]([OH:11])[CH:9]=1

参加物

3

反応物 1

HCID 178470035HCID 178470035、化合物

生成物 1

HCID 178516647HCID 178516647、化合物収率 99.5%

試薬・触媒・溶媒 1

HCID 313Hydrochloric Acid溶媒

反応条件

温度
100 °C

実験手順

2,4-Dihydroxy-6-trifluoromethyl-nicotinic acid ethyl ester (62 g/247 mmol) was added in several portions over 30 min to 6M HCl(aq) (620 mL) at reflux. Heated at 100° C. overnight with vigorous stirring to obtain complete solution. Allowed to cool and concentrated in vacuo to a white solid. Slurried in water (250 mL) and adjusted to pH 7 with concentrated ammonia to get heavy white suspension. Collected solid by filtration, rinsing through with fresh water, and dried to provide 6-trifluoromethyl-pyridine-2,4-diol (44.0 g) as a white solid.

後処理

  1. temperatureat reflux
  2. customto obtain complete solution
  3. temperatureto cool
  4. concentrationconcentrated in vacuo to a white solid
  5. customto get heavy white suspension
  6. customCollected solid
  7. filtrationby filtration
  8. washrinsing through with fresh water
  9. customdried

出典と根拠

ORDレコード
ord-6c6927a6d71946c8831a739cf18d1414
出典データセット
uspto-grants-2013_02
特許番号
US08372836B2

関連ノート

読み込み中…