Potassium Carbonate → HCID 178429526, 화합물

HRID 577071노트

반응식

HRID 577071 반응식
Cl.[Cl:2][C:3]1[N:7]([CH3:8])[CH:6]=[N:5][C:4]=1[CH2:9]Cl.[CH3:11][C:12]1[N:17]=[C:16]([SH:18])[N:15]=[C:14]([OH:19])[CH:13]=1.C(=O)([O-])[O-].[K+].[K+]>CC(C)=O>[Cl:2][C:3]1[N:7]([CH3:8])[CH:6]=[N:5][C:4]=1[CH2:9][S:18][C:16]1[N:15]=[C:14]([OH:19])[CH:13]=[C:12]([CH3:11])[N:17]=1

참가 물질

5

반응물 3

HCID 11430Potassium CarbonateHCID 668208135-chloro-4-(chloromethyl)-1-methyl-1H-imidazole hydrochlorideHCID 178429541HCID 178429541, 화합물

생성물 1

HCID 178429526HCID 178429526, 화합물수율 246.2%

시약·촉매·용매 1

HCID 180Acetone용매

실험 절차

A mixture of 5-chloro-4-(chloromethyl)-1-methyl-1H-imidazole hydrochloride (463 mg, 2.3 mmol), 6-methyl-2-sulfanylpyrimidin-4-ol (213 mg, 1.5 mmol), and potassium carbonate (1.1 g, 8.0 mmol) in acetone (15 mL) was stirred at room temperature overnight. The solid material was removed by filtration and washed with 50% acetone/MeOH (2×15 mL). The filtrate was recovered and evaporated. The crude product was purified by flash chromatography (0-10% MeOH/DCM and 0-6% MeOH/DCM), affording 2-{[(5-chloro-1-methyl-1H-imidazol-4-yl)methyl]sulfanyl}-6-methylpyrimidin-4-ol (1.0 g, 93% yield); 1H NMR (400 MHz, DMSO-d6): δ 2.17 (s, 3H), 3.53 (s, 3H), 4.25 (s, 2H), 5.97 (s, 1H), 7.70 (s, 1H); M+271. The product was used without further purification.

후처리

  1. customThe solid material was removed by filtration
  2. washwashed with 50% acetone/MeOH (2×15 mL)
  3. customThe filtrate was recovered
  4. customevaporated
  5. customThe crude product was purified by flash chromatography (0-10% MeOH/DCM and 0-6% MeOH/DCM)

출처 및 근거

ORD 기록
ord-489cf0dd805341efb3fb9f4c98fd37f2
출처 데이터셋
uspto-grants-2015_05
특허 번호
US09040538B2

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