Sodium Bicarbonate → HCID 58012362、化合物

HRID 1698545ノート

反応式

HRID 1698545 の反応式
Cl[C:2]1[N:6]([CH3:7])[C:5]2[C:8]([C:12]3[CH:17]=[CH:16][CH:15]=[CH:14][C:13]=3[CH2:18][CH3:19])=[CH:9][CH:10]=[CH:11][C:4]=2[N:3]=1.[Br:20][C:21]1[CH:27]=[C:26]([CH3:28])[C:24]([NH2:25])=[C:23]([O:29][CH3:30])[CH:22]=1.C(=O)([O-])O.[Na+]>C(OCC)(=O)C>[Br:20][C:21]1[CH:27]=[C:26]([CH3:28])[C:24]([NH:25][C:2]2[N:6]([CH3:7])[C:5]3[C:8]([C:12]4[CH:17]=[CH:16][CH:15]=[CH:14][C:13]=4[CH2:18][CH3:19])=[CH:9][CH:10]=[CH:11][C:4]=3[N:3]=2)=[C:23]([O:29][CH3:30])[CH:22]=1

参加物

5

反応物 3

HCID 516892Sodium BicarbonateHCID 106802184-Bromo-2-methoxy-6-methylanilineHCID 67273043HCID 67273043、化合物

生成物 1

HCID 58012362HCID 58012362、化合物収率 54.2%

試薬・触媒・溶媒 1

HCID 8857Ethyl Acetate溶媒

反応条件

温度
120 °C

実験手順

A mixture of 100 mg (0.369 mmol) of 2-chloro-7-(2-ethylphenyl)-1-methyl-1H-benzimidazole and 239 mg (1.11 mmol) of 4-bromo-2-methoxy-6-methylaniline was stirred at 120° C. for 15 hours. After cooling, the reaction mixture was neutralized by saturated aqueous sodium hydrogen carbonate, followed by addition of ethyl acetate. The resulting crystals were collected by filtration and washed with water and ethyl acetate, and suspended in hot ethyl acetate. After cooling to room temperature, the crystals were collected by filtration and washed with ethyl acetate and a 50% dimethylsulfoxide/methanol mixture to give 90 mg (54%) of the title compound.

後処理

  1. temperatureAfter cooling
  2. filtrationThe resulting crystals were collected by filtration
  3. washwashed with water and ethyl acetate
  4. temperatureAfter cooling to room temperature
  5. filtrationthe crystals were collected by filtration
  6. washwashed with ethyl acetate

出典と根拠

ORDレコード
ord-28918a6c8bc64e0488f7d7a2fd6b6f38
出典データセット
uspto-grants-2012_04
特許番号
US08163935B2

反応ノート

読み込み中…