Hydrogen Peroxide → 2-Bromo-6-methoxyquinolin-3-ol

HRID 2045717노트

반응식

HRID 2045717 반응식
[OH:1]O.[Br:3][C:4]1[C:13](B(O)O)=[CH:12][C:11]2[C:6](=[CH:7][CH:8]=[C:9]([O:17][CH3:18])[CH:10]=2)[N:5]=1.[NH4+].[Cl-]>CCOCC.O>[Br:3][C:4]1[C:13]([OH:1])=[CH:12][C:11]2[C:6](=[CH:7][CH:8]=[C:9]([O:17][CH3:18])[CH:10]=2)[N:5]=1

참가 물질

6

반응물 3

HCID 784Hydrogen Peroxide2회HCID 25517Ammonium Chloride2회HCID 57416465(2-Bromo-6-methoxyquinolin-3-yl)boronic acid

생성물 1

HCID 580913652-Bromo-6-methoxyquinolin-3-ol수율 100%

시약·촉매·용매 2

HCID 962Water용매HCID 3283Diethyl Ether용매

실험 절차

Aqueous H2O2 (30%, 32.8 mL, 321 mmol) was added dropwise to a stirred solution of (2-bromo-6-methoxyquinolin-3-yl)boronic acid (4.64 g, 16.45 mmol) and NH4Cl (3.29 g, 61.5 mmol) in Et2O (82 mL) and water (82 mL). After 13 h, NH4Cl (3.29 g, 61.5 mmol) and aqueous H2O2 (30%, 32.8 mL, 321 mmol) were added, and the mixture was stirred for 48 h. The precipitate was collected and washed with water, then dried at 50° C. to afford the title compound (4.18 g, 100%) as a solid that was used directly in the subsequent step. LCMS (ES+) m/z 254, 256 (M+H)+,

후처리

  1. customThe precipitate was collected
  2. washwashed with water
  3. customdried at 50° C.

출처 및 근거

ORD 기록
ord-43d6af4d4a5844b0b73e0ab4b8c481a3
출처 데이터셋
uspto-grants-2013_11
특허 번호
US08591878B2

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