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

HRID 598073노트

반응식

HRID 598073 반응식
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]

참가 물질

5

반응물 2

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

생성물 1

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

시약·촉매·용매 2

HCID 962Water용매HCID 8028Tetrahydrofuran용매

반응 조건

온도
80 °C

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-628ed0411a0e4958b6f195fd11c0cd7c
출처 데이터셋
uspto-grants-2011_03
특허 번호
US07897607B2

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