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Potassium Carbonate → HCID 178462825, 화합물

HRID 630123
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HRID 630123 반응식
Cl.Cl[CH2:3][C:4]1[N:5]=[CH:6][N:7]([CH2:10][CH3:11])[C:8]=1[CH3:9].[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>[CH2:10]([N:7]1[C:8]([CH3:9])=[C:4]([CH2:3][S:19][C:17]2[N:16]=[C:15]([OH:20])[CH:14]=[C:13]([CH3:12])[N:18]=2)[N:5]=[CH:6]1)[CH3:11]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 11430Potassium CarbonateHCID 668207564-(chloromethyl)-1-ethyl-5-methyl-1H-imidazole hydrochlorideHCID 178429541HCID 178429541, 화합물

생성물 1

HCID 178462825HCID 178462825, 화합물수율 32.3%

시약·촉매·용매 1

HCID 180Acetone용매

실험 절차

A mixture of 4-(chloromethyl)-1-ethyl-5-methyl-1H-imidazole hydrochloride (450 mg, 2.3 mmol), 6-methyl-2-sulfanylpyrimidin-4-ol (215 mg, 1.5 mmol), and potassium carbonate (720 mg, 5.2 mmol) in acetone (15 mL) was stirred at room temperature for 3 days. 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-5-methyl-1H-imidazol-4-yl)methyl]sulfanyl}-6-methylpyrimidin-4-ol (128 mg, 32% yield); 1H NMR (400 MHz, DMSO-d6): δ 1.26 (t, 3H, J=6.7 Hz), 2.18 (m, 6H), 3.86 (m, 2H), 4.26 (s, 2H), 5.95 (s, 1H), 7.55 (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-0122a6825a144bf0b7b4b0510d29448c
출처 데이터셋
uspto-grants-2016_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09315521B2

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