Methane → HCID 178495389、化合物

HRID 888246ノート

反応式

HRID 888246 の反応式
[CH3:1][C:2]1[C:7]([CH2:8][S+:9]([O-:19])[C:10]2[NH:11][C:12]3[CH:13]=[CH:14][CH:15]=[CH:16][C:17]=3[N:18]=2)=[N:6][CH:5]=[CH:4][C:3]=1[O:20][CH2:21][CH2:22][CH2:23][O:24][CH3:25].[OH-].[Na+:27].C>C1COCC1>[CH3:1][C:2]1[C:7]([CH2:8][S+:9]([O-:19])[C:10]2[N-:11][C:12]3[CH:13]=[CH:14][CH:15]=[CH:16][C:17]=3[N:18]=2)=[N:6][CH:5]=[CH:4][C:3]=1[O:20][CH2:21][CH2:22][CH2:23][O:24][CH3:25].[Na+:27]

参加物

5

反応物 3

HCID 297MethaneHCID 14798Sodium HydroxideHCID 178495390HCID 178495390、化合物

生成物 1

HCID 178495389HCID 178495389、化合物

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

反応条件

温度
27.5 °C

実験手順

Rabeprazole (10 g) was suspended in 30 ml THF and sodium hydroxide solution (1.11 g sodium hydroxide dissolved in 1 ml water) was added at 25-30° C. Reaction mass was stirred for 30 minutes at 25-30° C. Added activated charcoal (1.0 g) and stirred for 30 minutes at 25-30° C. Filtered and washed charcoal bed with THF (20 ml). Distilled out THF under reduced pressure at 30-35° C. completely. Residue was dissolved in THF (20 ml). In a separate R B flask charged n-heptane (100 ml) at 25° C. Added slowly above reaction mass in 15-20 minutes at 25-30° C. Stirred at 25-30° C. for 2 hours. The product was filtered off under nitrogen atmosphere and wet cake was washed with n-heptane (2×20 ml). Dried under vacuum at 50° C. for 20-24 hours to obtain amorphous Rabeprazole sodium.

後処理

  1. customReaction mass
  2. stirringstirred for 30 minutes at 25-30° C
  3. filtrationFiltered
  4. washwashed charcoal bed with THF (20 ml)
  5. distillationDistilled out THF under reduced pressure at 30-35° C. completely
  6. dissolutionResidue was dissolved in THF (20 ml)
  7. additionIn a separate R B flask charged n-heptane (100 ml) at 25° C
  8. additionAdded slowly above reaction mass in 15-20 minutes at 25-30° C
  9. stirringStirred at 25-30° C. for 2 hours
  10. filtrationThe product was filtered off under nitrogen atmosphere
  11. washwet cake was washed with n-heptane (2×20 ml)
  12. customDried under vacuum at 50° C. for 20-24 hours

出典と根拠

ORDレコード
ord-bb104dbafb1644d49388e0661c3fddb6
出典データセット
uspto-grants-2012_08
特許番号
US08247568B2

反応ノート

読み込み中…