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Sodium Iodide → 7-benzyl-N-(4-(trifluoromethyl)phenyl)-5,6,7,8-tetrahydro-2-(methylthio)pyrido[3,4-d]pyrimidin-4-amine

HRID 2219951
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HRID 2219951 반응식
[I-].[Na+].I.[CH2:4]([N:11]1[CH2:20][CH2:19][C:18]2[C:17](Cl)=[N:16][C:15]([S:22][CH3:23])=[N:14][C:13]=2[CH2:12]1)[C:5]1[CH:10]=[CH:9][CH:8]=[CH:7][CH:6]=1.[NH2:24][C:25]1[CH:30]=[CH:29][C:28]([C:31]([F:34])([F:33])[F:32])=[CH:27][CH:26]=1>O1CCOCC1>[CH2:4]([N:11]1[CH2:20][CH2:19][C:18]2[C:17]([NH:24][C:25]3[CH:30]=[CH:29][C:28]([C:31]([F:32])([F:33])[F:34])=[CH:27][CH:26]=3)=[N:16][C:15]([S:22][CH3:23])=[N:14][C:13]=2[CH2:12]1)[C:5]1[CH:10]=[CH:9][CH:8]=[CH:7][CH:6]=1
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참가 물질

6

반응물 4

HCID 5238Sodium IodideHCID 99644-(Trifluoromethyl)anilineHCID 24841Hydrogen iodideHCID 529876597-Benzyl-4-chloro-2-(methylthio)-5,6,7,8-tetrahydropyrido[3,4-D]pyrimidine

생성물 1

HCID 590215717-benzyl-N-(4-(trifluoromethyl)phenyl)-5,6,7,8-tetrahydro-2-(methylthio)pyrido[3,4-d]pyrimidin-4-amine수율 73.3%

시약·촉매·용매 1

HCID 312751,4-Dioxane용매

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온도
100 °C

실험 절차

Sodium iodide (3.9 g, 26 mmol) and hydriodic acid (10 mL, 47% aqueous solution) were added to the solution of 7-benzyl-4-chloro-5,6,7,8-tetrahydro-2-(methylthio)pyrido[3,4-d]pyrimidine (8.0 g, 26 mmol) and 4-aminobenzotrifluoride (5.06 g, 0.031 mol) in dioxane (100 mL) and the reaction solution was stirred at 100° C. overnight. Solid thus formed was filtered out, washed by ethyl acetate and diethyl ether and dried in vacuo. Product was obtained as white needle solid (8.2 g, 73%).

후처리

  1. customSolid thus formed
  2. filtrationwas filtered out
  3. washwashed by ethyl acetate and diethyl ether
  4. customdried in vacuo

출처 및 근거

ORD 기록
ord-e9a2474877824807a9030762aed93698
출처 데이터셋
uspto-grants-2008_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07414131B2

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