Sodium Bicarbonate → Voriconazole

HRID 1099521노트

반응식

HRID 1099521 반응식
[CH3:1][C@H:2]([C@@:10]([OH:25])([C:17]1[CH:18]=[CH:19][C:20]([F:24])=[CH:21][C:22]=1[F:23])[CH2:11][N:12]1[N:16]=[CH:15][N:14]=[CH:13]1)[C:3]1[N:8]=[CH:7][N:6]=[CH:5][C:4]=1[F:9].[C@@]12(CS([O-])(=O)=O)C(C)(C)C(CC1)CC2=O.C(=O)(O)[O-].[Na+]>C(OCC)(=O)C>[CH3:1][C@H:2]([C@@:10]([OH:25])([C:17]1[CH:18]=[CH:19][C:20]([F:24])=[CH:21][C:22]=1[F:23])[CH2:11][N:12]1[N:16]=[CH:15][N:14]=[CH:13]1)[C:3]1[N:8]=[CH:7][N:6]=[CH:5][C:4]=1[F:9]

참가 물질

4

반응물 2

HCID 516892Sodium BicarbonateHCID 86626425Voriconazole (1R)-(-)-10-camphorsulfonate

생성물 1

HCID 71616Voriconazole수율 91.2%

시약·촉매·용매 1

HCID 8857Ethyl Acetate용매

실험 절차

Voriconazole (1R)-(−)-10-camphorsulfonate (6 g, 10.3 mmol) was suspended in ethyl acetate (18 ml) and treated slowly with aqueous saturated solution of sodium bicarbonate (14.4 ml). The mixture was stirred for 10 minutes and allowed to settle. The organic phase was separated and the aqueous phase was re-extracted with ethyl acetate (13.5 ml). The combined organic phases were washed with deionised water (1.8 ml), filtered through paper and concentrated under reduced pressure to give a white solid (3.28 g, 91.11% yield).

후처리

  1. customThe organic phase was separated
  2. extractionthe aqueous phase was re-extracted with ethyl acetate (13.5 ml)
  3. washThe combined organic phases were washed with deionised water (1.8 ml)
  4. filtrationfiltered through paper
  5. concentrationconcentrated under reduced pressure

출처 및 근거

ORD 기록
ord-2c5bf0f15f59488483a12cee9edf4d56
출처 데이터셋
uspto-grants-2012_03
특허 번호
US08143397B2

반응 노트

불러오는 중…