Ethyl Acetate → 5-Bromo-6-isoquinolinol

HRID 1887066ノート

反応式

HRID 1887066 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 compound 7 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 compound 9 as an off-white solid.

後処理

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

出典と根拠

ORDレコード
ord-e9b98aa86194466b96fdeebe219ae783
出典データセット
uspto-grants-2013_08
特許番号
US08501736B2

反応ノート

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