Methane → HCID 178495389, 화합물

HRID 888246노트

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HRID 888246 반응식
[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]

참가 물질

5

반응물 3

HCID 297MethaneHCID 14798Sodium HydroxideHCID 178495390HCID 178495390, 화합물

생성물 1

HCID 178495389HCID 178495389, 화합물

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

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온도
27.5 °C

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-bb104dbafb1644d49388e0661c3fddb6
출처 데이터셋
uspto-grants-2012_08
특허 번호
US08247568B2

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