Ethyl Acetate → 5-Bromo-6-isoquinolinol

HRID 2370717ノート

反応式

HRID 2370717 の反応式
[Br:1]Br.[OH:3][C:4]1[CH:5]=[C:6]2[C:11](=[CH:12][CH:13]=1)[CH:10]=[N:9][CH:8]=[CH:7]2.C(OCC)(=O)C>C(Cl)(Cl)Cl>[Br:1][C:5]1[C:4]([OH:3])=[CH:13][CH:12]=[C:11]2[C:6]=1[CH:7]=[CH:8][N:9]=[CH:10]2

参加物

5

反応物 3

HCID 8857Ethyl AcetateHCID 24408BromineHCID 135483582Isoquinolin-6-ol

生成物 1

HCID 1360928955-Bromo-6-isoquinolinol収率 88.4%

試薬・触媒・溶媒 1

HCID 6212Chloroform溶媒

実験手順

7.9 mL (19.18 g, 120 mmol) of bromine were added dropwise to a suspension of 17.42 g (120 mmol) of 6-hydroxy isoquinoline in 250 mL of chloroform at room temperature. After stirring for 2 h, ethyl acetate was added. The precipitate was filtered, washed with ethyl acetate and dried. Aqueous NaHCO3 solution was added carefully. The precipitate was filtered and washed with NaHCO3 solution until the filtrate had a pH of 8. Drying gave 23.78 g (88%) of 2 as an off-white solid.

後処理

  1. filtrationThe precipitate was filtered
  2. washwashed with ethyl acetate
  3. customdried
  4. additionAqueous NaHCO3 solution was added carefully
  5. filtrationThe precipitate was filtered
  6. washwashed with NaHCO3 solution until the filtrate
  7. customDrying

出典と根拠

ORDレコード
ord-ffc5ecd8c4a44461b1fc098e8b0f863b
出典データセット
uspto-grants-2014_04
特許番号
US08710228B2

反応ノート

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