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Methanol → 5-(thiophen-2-yl)pyrimidine-2,4(1H,3H)-dione

HRID 1661058
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HRID 1661058 반응식
C([O:8][C:9]1[N:14]=[C:13]([O:15]CC2C=CC=CC=2)[C:12]([C:23]2[S:24][CH:25]=[CH:26][CH:27]=2)=[CH:11][N:10]=1)C1C=CC=CC=1.I[Si](C)(C)C.CO>ClCCl>[S:24]1[CH:25]=[CH:26][CH:27]=[C:23]1[C:12]1[C:13](=[O:15])[NH:14][C:9](=[O:8])[NH:10][CH:11]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 887MethanolHCID 85247Trimethylsilyl iodideHCID 12118032,4-Bis(benzyloxy)-5-(thiophen-2-yl)pyrimidine

생성물 1

HCID 8190965-(thiophen-2-yl)pyrimidine-2,4(1H,3H)-dione수율 67.3%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

To a solution of 2,4-bis(benzyloxy)-5-(thiophen-2-yl)pyrimidine (Prep21, 20 g, 53.5 mol) in dry dichloromethane (400 ml), iodotrimethylsilane (28.8 g, 0.14 mol) was added at room temperature. The resulting solution was stirred for 3 hours. Then methanol was added, the precipitate was filtered and the solid was recrystallized with methanol twice, to afford 7 g of the title compound (y=67.3%)

후처리

  1. filtrationthe precipitate was filtered
  2. customthe solid was recrystallized with methanol twice

출처 및 근거

ORD 기록
ord-55783d39b8ab4b05beb31932ffdd20fc
출처 데이터셋
uspto-grants-2011_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08030322B2

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