Acetic Acid → HCID 21979852、化合物

HRID 10536ノート

反応式

HRID 10536 の反応式
[CH3:1][S:2][C:3]1[C:12]2[C:7](=[CH:8][CH:9]=[CH:10][C:11]=2[NH:13][CH:14]2[CH2:19][CH2:18][N:17]([C:20]([O:22][C:23]([CH3:26])([CH3:25])[CH3:24])=[O:21])[CH2:16][CH2:15]2)[CH:6]=[N:5][CH:4]=1.C(O)(=[O:29])C.OO>C(OCC)(=O)C>[CH3:1][S:2]([C:3]1[C:12]2[C:7](=[CH:8][CH:9]=[CH:10][C:11]=2[NH:13][CH:14]2[CH2:15][CH2:16][N:17]([C:20]([O:22][C:23]([CH3:26])([CH3:25])[CH3:24])=[O:21])[CH2:18][CH2:19]2)[CH:6]=[N:5][CH:4]=1)=[O:29]

参加物

5

反応物 3

HCID 176Acetic AcidHCID 784Hydrogen PeroxideHCID 21979971HCID 21979971、化合物

生成物 1

HCID 21979852HCID 21979852、化合物

試薬・触媒・溶媒 1

HCID 8857Ethyl Acetate溶媒

実験手順

Intermediate 74 (746 mg) obtained in Example 105, Step B was added with acetic acid (1.5 ml) and 30% aqueous hydrogen peroxide (2 ml) and stirred at room temperature for 17 hours. The reaction mixture was added with ethyl acetate (50 ml) and washed three times with saturated aqueous sodium hydrogencarbonate (25 ml for each time), and the organic layer was dried over anhydrous sodium sulfate. The solvent was evaporated under reduced pressure, and the residue was purified by silica gel column chromatography (n-hexane:acetone=3:1) to obtain the title compound (390 mg).

後処理

  1. washwashed three times with saturated aqueous sodium hydrogencarbonate (25 ml for each time), and the organic layer
  2. dry with materialwas dried over anhydrous sodium sulfate
  3. customThe solvent was evaporated under reduced pressure
  4. customthe residue was purified by silica gel column chromatography (n-hexane:acetone=3:1)

出典と根拠

ORDレコード
ord-43fad62811f54559b279903164b86c04
出典データセット
uspto-grants-2006_08
特許番号
US07094789B2

反応ノート

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