Perboric acid, sodium salt, monohydrate → HCID 68815368, 화합물

HRID 732436노트

반응식

HRID 732436 반응식
B(O[O-])=O.[OH2:5].[Na+].[CH3:7][O:8][C:9](=[O:25])[C:10]1[CH:15]=[C:14]([S:16][CH2:17][CH2:18][CH3:19])[N:13]=[C:12]([NH:20][C@H:21]([CH2:23][CH3:24])[CH3:22])[CH:11]=1>C(O)(=O)C>[CH3:7][O:8][C:9](=[O:25])[C:10]1[CH:15]=[C:14]([S@:16]([CH2:17][CH2:18][CH3:19])=[O:5])[N:13]=[C:12]([NH:20][CH:21]([CH2:23][CH3:24])[CH3:22])[CH:11]=1

참가 물질

4

반응물 2

HCID 23695970Perboric acid, sodium salt, monohydrateHCID 68814642HCID 68814642, 화합물

생성물 1

HCID 68815368HCID 68815368, 화합물수율 58%

시약·촉매·용매 1

HCID 176Acetic Acid용매

실험 절차

Add sodium perborate monohydrate (0.133 g, 1.33 mmol) to a cooled solution of (S)-2-sec-butylamino-6-propylsulfanyl-isonicotinic acid methyl ester (0.396 g, 1.40 mmol) in acetic acid (4 mL). Stir at room temperature overnight and concentrate. Dissolve the residue in ethyl acetate and wash the solution with aqueous sodium bicarbonate, saturated aqueous sodium chloride, dry (magnesium sulfate), concentrate and purify (silica gel chromatography, eluting with 30:70 ethyl acetate:hexanes) to give the title compound (0.230 g, 55%).

후처리

  1. concentrationconcentrate
  2. dissolutionDissolve the residue in ethyl acetate
  3. washwash the solution with aqueous sodium bicarbonate, saturated aqueous sodium chloride
  4. dry with materialdry (magnesium sulfate)
  5. concentrationconcentrate
  6. custompurify
  7. wash(silica gel chromatography, eluting with 30:70 ethyl acetate:hexanes)

출처 및 근거

ORD 기록
ord-9e4ac74249144bb488860c078f4a9688
출처 데이터셋
uspto-grants-2009_09
특허 번호
US07585885B2

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