Hydrochloric Acid → Methyl 6-(4-(ethylsulfonyl)phenoxy)-2-pyridin-2-yl-1H-benzimidazole-5-carboxylate

HRID 1671664ノート

反応式

HRID 1671664 の反応式
[CH2:1]([S:3]([C:6]1[CH:34]=[CH:33][C:9]([O:10][C:11]2[CH:20]=[C:19]([NH:21][C:22]([C:24]3[CH:29]=[CH:28][CH:27]=[CH:26][N:25]=3)=O)[C:18]([N+:30]([O-])=O)=[CH:17][C:12]=2[C:13]([O:15][CH3:16])=[O:14])=[CH:8][CH:7]=1)(=[O:5])=[O:4])[CH3:2].O.O.[Sn](Cl)Cl.Cl.C(=O)([O-])O.[Na+]>CN(C)C=O.CO.C(OCC)(=O)C>[CH2:1]([S:3]([C:6]1[CH:34]=[CH:33][C:9]([O:10][C:11]2[C:12]([C:13]([O:15][CH3:16])=[O:14])=[CH:17][C:18]3[NH:30][C:22]([C:24]4[CH:29]=[CH:28][CH:27]=[CH:26][N:25]=4)=[N:21][C:19]=3[CH:20]=2)=[CH:8][CH:7]=1)(=[O:4])=[O:5])[CH3:2]

参加物

8

反応物 4

HCID 313Hydrochloric AcidHCID 61436Stannous chloride dihydrateHCID 516892Sodium BicarbonateHCID 57433541Methyl 2-[4-(ethylsulfonyl)phenoxy]-5-nitro-4-[(2-pyridinylcarbonyl)amino]benzoate

生成物 1

HCID 57433643Methyl 6-(4-(ethylsulfonyl)phenoxy)-2-pyridin-2-yl-1H-benzimidazole-5-carboxylate

試薬・触媒・溶媒 3

HCID 887Methanol溶媒HCID 6228Dimethylformamide溶媒HCID 8857Ethyl Acetate溶媒

反応条件

温度
80 °C

実験手順

Methyl 2-[4-(ethylsulfonyl)phenoxy]-5-nitro-4-[(2-pyridinylcarbonyl)amino]benzoate (7.46 g) was suspended in dimethylformamide (37 ml) and methanol (37 ml), and tin(II) chloride dihydrate (17.3 g) and concentrated hydrochloric acid (15 ml) were added to it, and stirred under heat at 80° C. for 40 minutes. The reaction liquid was restored to room temperature, and gradually added to an aqueous sodium hydrogencarbonate solution and neutralized. Ethyl acetate was added to it, and stirred at room temperature for 30 minutes, and the formed salt was taken out through filtration. The filtrate was washed with water and saturated saline water. After dried, the solvent was evaporated away to obtain the entitled compound as a yellow solid.

後処理

  1. customThe reaction liquid
  2. customwas restored to room temperature
  3. stirringstirred at room temperature for 30 minutes
  4. filtrationthe formed salt was taken out through filtration
  5. washThe filtrate was washed with water and saturated saline water
  6. customAfter dried
  7. customthe solvent was evaporated away

出典と根拠

ORDレコード
ord-efce8ba978f24b90b5aa16abeb002c00
出典データセット
uspto-grants-2011_08
特許番号
US07994331B2

反応ノート

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