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Potassium Carbonate → HCID 178462821, 화합물

HRID 630118
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HRID 630118 반응식
Cl.Cl[CH2:3][C:4]1[N:8]([CH2:9][CH3:10])[CH:7]=[N:6][C:5]=1[CH3:11].[CH3:12][C:13]1[N:18]=[C:17]([SH:19])[N:16]=[C:15]([OH:20])[CH:14]=1.C(=O)([O-])[O-].[K+].[K+]>CC(C)=O>[CH2:9]([N:8]1[C:4]([CH2:3][S:19][C:17]2[N:16]=[C:15]([OH:20])[CH:14]=[C:13]([CH3:12])[N:18]=2)=[C:5]([CH3:11])[N:6]=[CH:7]1)[CH3:10]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 11430Potassium CarbonateHCID 668206265-(chloromethyl)-1-ethyl-4-methyl-1H-imidazole hydrochlorideHCID 178429541HCID 178429541, 화합물

생성물 1

HCID 178462821HCID 178462821, 화합물수율 46.3%

시약·촉매·용매 1

HCID 180Acetone용매

실험 절차

A mixture of 5-(chloromethyl)-1-ethyl-4-methyl-1H-imidazole hydrochloride (1.0 g, 5.1 mmol), 6-methyl-2-sulfanylpyrimidin-4-ol (500 mg, 3.5 mmol), and potassium carbonate (1.2 g, 9.0 mmol) in acetone (25 mL) was stirred at room temperature overnight. The solid material was removed by filtration. The filtrate was recovered and evaporated. The crude product was purified by flash chromatography (0-6% MeOH/DCM), affording 2-{[(1-ethyl-4-methyl-1H-imidazol-5-yl)methyl]sulfanyl}-6-methyl-pyrimidin-4-ol (428 mg, 46% yield); 1H NMR (400 MHz, DMSO-d6): δ 1.31 (t, 3H, J=6.7 Hz), 2.11 (s, 3H), 2.22 (s, 3H), 3.95 (m, 2H), 4.48 (s, 2H), 6.02 (s, 1H), 7.54 (s, 1H); M+266. The product was used without further purification.

후처리

  1. customThe solid material was removed by filtration
  2. customThe filtrate was recovered
  3. customevaporated
  4. customThe crude product was purified by flash chromatography (0-6% MeOH/DCM)

출처 및 근거

ORD 기록
ord-509eb9c2ddb54dbf9e633ca48c8f944b
출처 데이터셋
uspto-grants-2016_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09315521B2

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