Acetic Acid → 2-methylsulfanyl-3H-thieno[2,3-d]pyrimidin-4-one

HRID 9768

반응식

HRID 9768 반응식
[S:1]=[C:2]1[NH:7][C:6]2[S:8][CH:9]=[CH:10][C:5]=2[C:4](=[O:11])[NH:3]1.CI.[C:14](O)(=O)C>[OH-].[Na+]>[CH3:14][S:1][C:2]1[NH:3][C:4](=[O:11])[C:5]2[CH:10]=[CH:9][S:8][C:6]=2[N:7]=1

참가 물질

5

반응물 3

HCID 176Acetic AcidHCID 6328Methyl iodideHCID 36033932-sulfanyl-3H,4H-thieno(2,3-d)pyrimidin-4-one

생성물 1

HCID 38520912-methylsulfanyl-3H-thieno[2,3-d]pyrimidin-4-one

시약·촉매·용매 1

HCID 14798Sodium Hydroxide용매

반응 조건

온도
0 °C

실험 절차

To a solution of 2-thioxo-2,3-dihydro-1H-thieno[2,3-d]pyrimidin-4-one (25.4 g, 0.138 mol) in 1N aqueous NaOH (600 mL) at room temperature was added methyl iodide (10.3 mL, 1.2 eq). The resulting mixture was stirred vigorously for about 2.5 hours. The reaction mixture was cooled to 0° C. and acetic acid was added (about 80 mL) until about pH=4.5 was reached. A fine precipitate was filtered and dried overnight to afford the title compound as a fine tan powder (24.8 g) (M+=198, M.P.=231.6–235.0° C.).

후처리

  1. filtrationA fine precipitate was filtered
  2. customdried overnight

출처 및 근거

ORD 기록
ord-53c7f10c5ffc4baebb47a80de51c29b8
출처 데이터셋
uspto-grants-2006_08
특허 번호
US07091347B2

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