Ethyl Acetate → 5-Bromo-6-isoquinolinol

HRID 2370717노트

반응식

HRID 2370717 반응식
[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

참가 물질

5

반응물 3

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

생성물 1

HCID 1360928955-Bromo-6-isoquinolinol수율 88.4%

시약·촉매·용매 1

HCID 6212Chloroform용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-ffc5ecd8c4a44461b1fc098e8b0f863b
출처 데이터셋
uspto-grants-2014_04
특허 번호
US08710228B2

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