Acetic Acid → HCID 178488154、化合物

HRID 1922003ノート

反応式

HRID 1922003 の反応式
[K].[CH3:2][O:3][C:4]1[CH:25]=[CH:24][C:7]2[NH:8][C:9]([S:11]([CH2:13][C:14]3[C:19]([CH3:20])=[C:18]([O:21][CH3:22])[C:17]([CH3:23])=[CH:16][N:15]=3)=[O:12])=[N:10][C:6]=2[CH:5]=1.C(O)(=O)C.CO.O.O.O.O.O.O.[Cl-].[Mg+2:39].[Cl-]>O>[Mg:39].[CH3:2][O:3][C:4]1[CH:25]=[CH:24][C:7]2[NH:8][C:9]([S:11]([CH2:13][C:14]3[C:19]([CH3:20])=[C:18]([O:21][CH3:22])[C:17]([CH3:23])=[CH:16][N:15]=3)=[O:12])=[N:10][C:6]=2[CH:5]=1

参加物

6

反応物 4

HCID 176Acetic AcidHCID 887MethanolHCID 24644Magnesium chloride hexahydrateHCID 178488152HCID 178488152、化合物

生成物 1

HCID 178488154HCID 178488154、化合物

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

5-methoxy-2-[[(4-methoxy-3,5-dimethyl-2-pyridinyl)-methyl]sulfinyl]-1H-benzimidazole potassium salt (100 g) was taken in water (500 ml) and was stirred at room temperature for 10-15 minutes. The pH was adjusted to 10-11 with acetic acid at and the mixture was stirred for half an hour 20-25° C. Methanol (100 ml) was added. Aqueous solution of magnesium chloride hexahydrate (20.3 g dissolved in 100 ml) was then added to the above mixture at room temperature under stirring. The mixture was stirred for 60 minutes at room temperature. The resulting solid was filtered, washed with methanol and water. The wet material was dried under reduced pressure at 40-45° C. for 8-10 hours.

後処理

  1. stirringwas stirred for half an hour 20-25° C
  2. stirringunder stirring
  3. stirringThe mixture was stirred for 60 minutes at room temperature
  4. filtrationThe resulting solid was filtered
  5. washwashed with methanol and water
  6. customThe wet material was dried under reduced pressure at 40-45° C. for 8-10 hours

出典と根拠

ORDレコード
ord-d595064cd1fe486d8f9ba3431663a230
出典データセット
uspto-grants-2012_05
特許番号
US08173818B2

反応ノート

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