Sodium Hydroxide → 2-chloro-7-methoxy-8-methyl-1H-quinazolin-4-one

HRID 1443490노트

반응식

HRID 1443490 반응식
[OH-:1].[Na+].[Cl:3][C:4]1[N:13]=[C:12](Cl)[C:11]2[C:6](=[C:7]([CH3:17])[C:8]([O:15][CH3:16])=[CH:9][CH:10]=2)[N:5]=1>O.C1COCC1>[Cl:3][C:4]1[N:13]=[C:12]([OH:1])[C:11]2[C:6](=[C:7]([CH3:17])[C:8]([O:15][CH3:16])=[CH:9][CH:10]=2)[N:5]=1

참가 물질

5

반응물 2

HCID 14798Sodium HydroxideHCID 591654322,4-Dichloro-7-methoxy-8-methylquinazoline

생성물 1

HCID 1784877522-chloro-7-methoxy-8-methyl-1H-quinazolin-4-one수율 99.3%

시약·촉매·용매 2

HCID 962Water용매HCID 8028Tetrahydrofuran용매

반응 조건

온도
40 °C

실험 절차

A solution of NaOH (1.58 g, 39.6 mmol) in water (40 mL) was added to 2,4-dichloro-7-methoxy-8-methylquinazoline (139) (3.2 g, 13.05 mmol) in THF (20 mL). The resulting mixture was heated at 40° C. for 24 h. Then, the reaction mixture was cooled to room temperature, THF was evaporated and additional water (30 mL) was added. The precipitate was filtered off. Then, the pH of the filtrate was adjusted to 5 with AcOH to give a solid which was subsequently filtered off and successively washed with water and isopropylether to give the title compound (2.91 g, 99%) as a yellowish powder: m/z=225 (M+H)+.

후처리

  1. temperatureThen, the reaction mixture was cooled to room temperature
  2. customTHF was evaporated
  3. additionadditional water (30 mL) was added
  4. filtrationThe precipitate was filtered off
  5. customto give a solid which
  6. filtrationwas subsequently filtered off
  7. washsuccessively washed with water and isopropylether

출처 및 근거

ORD 기록
ord-3ebf83711de04fe6829a5b30fbc2ae75
출처 데이터셋
uspto-grants-2010_02
특허 번호
US07659245B2

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