Potassium Carbonate → 6-(6-chloropyrimidin-4-yloxy)-2-(methoxymethyl)-4-methyl-1H-benzo[d]imidazole

HRID 1846466노트

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HRID 1846466 반응식
[CH3:1][O:2][CH2:3][C:4]1[NH:8][C:7]2[CH:9]=[C:10]([OH:14])[CH:11]=[C:12]([CH3:13])[C:6]=2[N:5]=1.[Cl:15][C:16]1[CH:21]=[C:20](Cl)[N:19]=[CH:18][N:17]=1.C(=O)([O-])[O-].[K+].[K+]>CN(C=O)C>[Cl:15][C:16]1[N:17]=[CH:18][N:19]=[C:20]([O:14][C:10]2[CH:11]=[C:12]([CH3:13])[C:6]3[N:5]=[C:4]([CH2:3][O:2][CH3:1])[NH:8][C:7]=3[CH:9]=2)[CH:21]=1

참가 물질

5

반응물 3

HCID 11430Potassium CarbonateHCID 709434,6-DichloropyrimidineHCID 669782392-(methoxymethyl)-4-methyl-1H-benzo[d]imidazol-6-ol

생성물 1

HCID 866639136-(6-chloropyrimidin-4-yloxy)-2-(methoxymethyl)-4-methyl-1H-benzo[d]imidazole

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

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온도
70 °C

실험 절차

0.77 g (4.00 mmol) 2-(methoxymethyl)-4-methyl-1H-benzo[d]imidazol-6-ol and 0.68 g (4.40 mmol) 4,6-dichloropyrimidine in 5.0 mL DMF were combined with 1.66 g (12.0 mmol) potassium carbonate and stirred for 8 h at 70° C. Then ice water was added and the substance was extracted with ethyl acetate and concentrated by rotary evaporation i.vac. The residue was purified by preparative HPLC-MS. The fractions containing product were combined and evaporated down i.vac.

후처리

  1. extractionthe substance was extracted with ethyl acetate
  2. concentrationconcentrated by rotary evaporation i.vac
  3. customThe residue was purified by preparative HPLC-MS
  4. additionThe fractions containing product
  5. customevaporated down i.vac

출처 및 근거

ORD 기록
ord-55f5ac9dc65742c381a3894364a0fbee
출처 데이터셋
uspto-grants-2015_02
특허 번호
US08952014B2

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