Acetic Acid → Lansoprazole

HRID 394825

反応式

HRID 394825 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][C:10]([F:13])([F:12])[F:11].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:7]([O:8][CH2:9][C:10]([F:12])([F:11])[F:13])=[CH:6][CH:5]=[N:4][C:3]=1[CH2:14][S+:15]([O-:26])[C:16]1[NH:20][C:19]2[CH:21]=[CH:22][CH:23]=[CH:24][C:18]=2[N:17]=1

参加物

7

反応物 4

HCID 176Acetic AcidHCID 962WaterHCID 159762Sodium percarbonateHCID 1094080Lansoprazole sulfide

生成物 1

HCID 3883Lansoprazole収率 238.6%

試薬・触媒・溶媒 2

HCID 61578Diammonium molybdate触媒HCID 887Methanol溶媒

反応条件

温度
10 °C

実験手順

10 g of 2-[[[3-methyl-4-(2,2,2-trifluoroethoxy)-2-pyridinyl]methyl]thio]-1H-benzimidazol were dissolved in 50 ml of methanol and 0.3 g of ammonium molybdate were added. The solution was cooled to 10° C., and 3.35 g of sodium percarbonate added slowly, kept stirred at the same temperature for 15 hours. After the reaction ended 250 ml of water were added and the pH of the resulting mixture adjusted to 10 with 10% acetic acid. This was kept stirred for 1 hour and the solid obtained was filtered, and subsequently washed with water and dried in a vacuum oven at 40° C. This provided 9.4 g of lansoprazol (yield: 90%).

後処理

  1. additionwere added
  2. stirringThis was kept stirred for 1 hour
  3. customthe solid obtained
  4. filtrationwas filtered
  5. washsubsequently washed with water
  6. customdried in a vacuum oven at 40° C

出典と根拠

ORDレコード
ord-858f083ce39e4c66a135dc371a8ec34e
出典データセット
uspto-grants-2003_08
特許番号
US06603009B2

関連ノート

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