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

HRID 1846466ノート

反応式

HRID 1846466 の反応式
[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

参加物

5

反応物 3

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

反応条件

温度
70 °C

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-55f5ac9dc65742c381a3894364a0fbee
出典データセット
uspto-grants-2015_02
特許番号
US08952014B2

反応ノート

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