Dipropylamine → 2-Dipropylamino-5-methoxy-3-methylquinazolin-4(3H)-one

HRID 598073ノート

反応式

HRID 598073 の反応式
Cl[C:2]1[N:11]([CH3:12])[C:10](=[O:13])[C:9]2[C:4](=[CH:5][CH:6]=[CH:7][C:8]=2[O:14][CH3:15])[N:3]=1.[CH2:16]([NH:19][CH2:20][CH2:21][CH3:22])[CH2:17][CH3:18]>O1CCCC1.O>[CH2:16]([N:19]([CH2:20][CH2:21][CH3:22])[C:2]1[N:11]([CH3:12])[C:10](=[O:13])[C:9]2[C:4](=[CH:5][CH:6]=[CH:7][C:8]=2[O:14][CH3:15])[N:3]=1)[CH2:17][CH3:18]

参加物

5

反応物 2

HCID 8902DipropylamineHCID 672666982-Chloro-5-methoxy-3-methylquinazolin-4(3H)-one

生成物 1

HCID 672671382-Dipropylamino-5-methoxy-3-methylquinazolin-4(3H)-one収率 45.5%

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 8028Tetrahydrofuran溶媒

反応条件

温度
80 °C

実験手順

A mixture of 2-chloro-5-methoxy-3-methylquinazolin-4(3H)-one (75 mg, 0.334 mmol) and dipropylamine (0.137 ml, 1.00 mmol) in tetrahydrofuran (1 ml) was stirred at 80° C. for 60 h and diluted with water. The aqueous solution was extracted with ethyl acetate. The extract was washed with brine, dried over magnesium sulfate and concentrated under vacuum. The residue was purified by column chromatography eluting with 50% ethyl acetate/n-hexane to afford 44 mg (45%) of the title compound.

後処理

  1. extractionThe aqueous solution was extracted with ethyl acetate
  2. washThe extract was washed with brine
  3. dry with materialdried over magnesium sulfate
  4. concentrationconcentrated under vacuum
  5. customThe residue was purified by column chromatography
  6. washeluting with 50% ethyl acetate/n-hexane

出典と根拠

ORDレコード
ord-628ed0411a0e4958b6f195fd11c0cd7c
出典データセット
uspto-grants-2011_03
特許番号
US07897607B2

反応ノート

読み込み中…