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

HRID 2045717ノート

反応式

HRID 2045717 の反応式
[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

参加物

6

反応物 3

HCID 784Hydrogen Peroxide2 回HCID 25517Ammonium Chloride2 回HCID 57416465(2-Bromo-6-methoxyquinolin-3-yl)boronic acid

生成物 1

HCID 580913652-Bromo-6-methoxyquinolin-3-ol収率 100%

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 3283Diethyl Ether溶媒

実験手順

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)+,

後処理

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

出典と根拠

ORDレコード
ord-43d6af4d4a5844b0b73e0ab4b8c481a3
出典データセット
uspto-grants-2013_11
特許番号
US08591878B2

反応ノート

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