Acetic Acid → HCID 21979852, 화합물

HRID 10536노트

반응식

HRID 10536 반응식
[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]

참가 물질

5

반응물 3

HCID 176Acetic AcidHCID 784Hydrogen PeroxideHCID 21979971HCID 21979971, 화합물

생성물 1

HCID 21979852HCID 21979852, 화합물

시약·촉매·용매 1

HCID 8857Ethyl Acetate용매

실험 절차

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).

후처리

  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)

출처 및 근거

ORD 기록
ord-43fad62811f54559b279903164b86c04
출처 데이터셋
uspto-grants-2006_08
특허 번호
US07094789B2

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