Perboric acid, sodium salt, monohydrate → HCID 68815368、化合物

HRID 732436ノート

反応式

HRID 732436 の反応式
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

参加物

4

反応物 2

HCID 23695970Perboric acid, sodium salt, monohydrateHCID 68814642HCID 68814642、化合物

生成物 1

HCID 68815368HCID 68815368、化合物収率 58%

試薬・触媒・溶媒 1

HCID 176Acetic Acid溶媒

実験手順

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%).

後処理

  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)

出典と根拠

ORDレコード
ord-9e4ac74249144bb488860c078f4a9688
出典データセット
uspto-grants-2009_09
特許番号
US07585885B2

反応ノート

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