Acetic Acid → HCID 178495390、化合物

HRID 394826ノート

反応式

HRID 394826 の反応式
[CH3:1][C:2]1[C:3]([CH2:14][S:15][C:16]2[NH:20][C:19]3[CH:21]=[CH:22][CH:23]=[CH:24][C:18]=3[N:17]=2)=[N:4][CH:5]=[CH:6][C:7]=1[O:8][CH2:9][CH2:10][CH2:11][O:12][CH3:13].C([O-])([O-])=[O:26].C([O-])([O-])=O.OO.OO.OO.[Na+].[Na+].[Na+].[Na+].O.C(O)(=O)C>CO.[NH4+].[NH4+].[O-][Mo]([O-])(=O)=O>[CH3:1][C:2]1[C:3]([CH2:14][S+:15]([O-:26])[C:16]2[NH:20][C:19]3[CH:21]=[CH:22][CH:23]=[CH:24][C:18]=3[N:17]=2)=[N:4][CH:5]=[CH:6][C:7]=1[O:8][CH2:9][CH2:10][CH2:11][O:12][CH3:13]

参加物

7

反応物 4

HCID 176Acetic AcidHCID 962WaterHCID 159762Sodium percarbonateHCID 9949996Rabeprazole-thioether

生成物 1

HCID 178495390HCID 178495390、化合物収率 200.8%

試薬・触媒・溶媒 2

HCID 61578Diammonium molybdate触媒HCID 887Methanol溶媒

反応条件

温度
5 °C

実験手順

2.3 g of 2-[[[3-methyl-4-(3-methoxypropoxy)-2-pyridinyl]methyl]thio]-1H-benzimidazol were dissolved in 11.5 ml of methanol and 90 mg of ammonium molybdate were added. The solution was cooled to 5° C. and 0.87 g of sodium percarbonate were added, then kept stirred at this temperature for 6 h. After the reaction finished 22 ml of water were added, then heating to 20° C. and adjusting the pH of the mixture to 7.5 with acetic acid. The mixture is extracted with 50 ml of dichloromethane and the organic phase was separated, which was then washed with 100 ml of water. The solvent was evaporated at a reduced pressure. 2.0 g of rabeprazol were obtained (yield: 81%).

後処理

  1. additionwere added
  2. temperatureheating to 20° C.
  3. extractionThe mixture is extracted with 50 ml of dichloromethane
  4. customthe organic phase was separated
  5. washwhich was then washed with 100 ml of water
  6. customThe solvent was evaporated at a reduced pressure

出典と根拠

ORDレコード
ord-829b935ad71c4a469b1fe5253629418b
出典データセット
uspto-grants-2003_08
特許番号
US06603009B2

反応ノート

読み込み中…