Sodium ethoxide → HCID 178467466、化合物

HRID 1443498ノート

反応式

HRID 1443498 の反応式
Cl[C:2]1[N:11]=[C:10]([OH:12])[C:9]2[C:4](=[C:5]([CH3:15])[C:6]([O:13][CH3:14])=[CH:7][CH:8]=2)[N:3]=1.[CH3:16][CH2:17][O-:18].[Na+]>>[CH2:17]([O:18][C:2]1[N:11]=[C:10]([OH:12])[C:9]2[C:4](=[C:5]([CH3:15])[C:6]([O:13][CH3:14])=[CH:7][CH:8]=2)[N:3]=1)[CH3:16]

参加物

3

反応物 2

HCID 2723922Sodium ethoxideHCID 1784877522-chloro-7-methoxy-8-methyl-1H-quinazolin-4-one

生成物 1

HCID 178467466HCID 178467466、化合物収率 96.6%

実験手順

The quinazolinol (140) (530 mg, 2.36 mmol) was added in small portions to freshly prepared EtONa (740 mg of Na added in 20 mL EtOH). The resulting solution was heated to reflux and after 24 h, the reaction mixture was cooled down to room temperature and evaporated. The residue was re-dissolved in water (10 mL) and the pH of the resulting solution was adjusted to 5 with AcOH. The precipitate was collected by filtration, washed with ice-cooled water and dried to give the title compound (534 mg, 96.6%) as a white solid, m/z=235 (M+H)+.

後処理

  1. temperatureThe resulting solution was heated
  2. temperatureto reflux and after 24 h
  3. customevaporated
  4. dissolutionThe residue was re-dissolved in water (10 mL)
  5. filtrationThe precipitate was collected by filtration
  6. washwashed with ice-
  7. temperaturecooled water
  8. customdried

出典と根拠

ORDレコード
ord-b0960885231f4f5da26cb26d835e2109
出典データセット
uspto-grants-2010_02
特許番号
US07659245B2

反応ノート

読み込み中…