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Magnesium Bromide → 5-hydroxy-7-methoxyquinazolin-4(3H)-one

HRID 1917792
ノート
印刷プレビュー

反応式

HRID 1917792 の反応式
C[O:2][C:3]1[CH:12]=[C:11]([O:13][CH3:14])[CH:10]=[C:9]2[C:4]=1[C:5](=[O:15])[NH:6][CH:7]=[N:8]2.[Mg+2].[Br-].[Br-]>N1C=CC=CC=1>[OH:2][C:3]1[CH:12]=[C:11]([O:13][CH3:14])[CH:10]=[C:9]2[C:4]=1[C:5](=[O:15])[NH:6][CH:7]=[N:8]2
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 82241Magnesium BromideHCID 1355106675,7-dimethoxyquinazolin-4(3H)-one

生成物 1

HCID 1355106955-hydroxy-7-methoxyquinazolin-4(3H)-one収率 98.2%

試薬・触媒・溶媒 1

HCID 1049Pyridine溶媒

実験手順

To a mixture of 5,7-dimethoxyquinazolin-4(3H)-one (4.80 g, 23.3 mmol) in pyridine (50 mL) at room temperature was slowly added MgBr2 (4.29 g, 23.3 mmol). It was heated to reflux for 1.5 hour. After solvent was evaporated under reduced pressure, to the residue was added a solution of AcOH (10 mL) in water (50 mL). A solid was precipitated. It was filtered, washed with water, and dried under vacuum with P2O5 to afford 5-hydroxy-7-methoxyquinazolin-4(3H)-one as solid (4.398 g, 98%). 1H NMR (300 MHz, DMSO-d6) δ 11.95 (br, 1H), 8.08 (s, 1H), 6.63 (s, 1H), 6.50 (s, 1H), 3.85 (s, 3H); LC-MS (ESI) m/z 193 (M+H)+.

後処理

  1. temperatureIt was heated
  2. temperatureto reflux for 1.5 hour
  3. customAfter solvent was evaporated under reduced pressure, to the residue
  4. additionwas added a solution of AcOH (10 mL) in water (50 mL)
  5. customA solid was precipitated
  6. filtrationIt was filtered
  7. washwashed with water
  8. dry with materialdried under vacuum with P2O5

出典と根拠

ORDレコード
ord-9a91ae0fd7714dc684e84fc29bf2779c
出典データセット
uspto-grants-2013_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08618289B2

反応ノート

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