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Acetic Acid → HCID 135967941, 화합물

HRID 1798808
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HRID 1798808 반응식
Cl.NO.[OH-].[Na+].C(O)(=O)C.C[N:11](/[CH:13]=[N:14]/[C:15](=[O:23])[C:16]1[CH:21]=[CH:20][C:19]([OH:22])=[CH:18][CH:17]=1)C>O1CCOCC1>[O:23]1[C:15]([C:16]2[CH:21]=[CH:20][C:19]([OH:22])=[CH:18][CH:17]=2)=[N:14][CH:13]=[N:11]1
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참가 물질

6

반응물 4

HCID 176Acetic AcidHCID 14798Sodium HydroxideHCID 443297Hydroxyamine hydrochlorideHCID 178484335HCID 178484335, 화합물

생성물 1

HCID 135967941HCID 135967941, 화합물

시약·촉매·용매 1

HCID 312751,4-Dioxane용매

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온도
90 °C

실험 절차

To a solution of hydroxylamine hydrochloride (354 mg, 5.1 mmol) in an a mixture of aqueous 5N sodium hydroxide solution (1 mL, 5 mmol), acetic acid (10 mL) and dioxane (8.5 mL) was added the N-[(1E)-(dimethylamino)methylene]-4-hydroxybenzamide from step 1 of this Example (815 mg, 4.24 mmol). The reaction was stirred at 90° C. for 3 hrs. Upon cooling to room temperature, the solvent was removed under vacuum and residue was purified by column chromatography on an 80 gram biotage silica gel cartridge eluting with 20-50% ethyl acetate/hexanes (gradient) to give the product as white solid. LRMS calc: 162.0; obs: 163.2 (M+1).

후처리

  1. temperatureUpon cooling to room temperature
  2. customthe solvent was removed under vacuum and residue
  3. customwas purified by column chromatography on an 80 gram biotage silica gel cartridge
  4. washeluting with 20-50% ethyl acetate/hexanes (gradient)

출처 및 근거

ORD 기록
ord-a1627fe981cc4c7b8f8c4df3dc75b45a
출처 데이터셋
uspto-grants-2013_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08343990B2

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