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

HRID 1436581노트

반응식

HRID 1436581 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-ddf5d54721e74993a2e19e2466e01013
출처 데이터셋
uspto-grants-2009_11
특허 번호
US07618978B2

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