Sodium Acetate → 2-Acetoxy-2-(4,6-dimethoxypyrimidin-2-yl)-N-methanesulfony-2-phenylacetamide

HRID 1451162노트

반응식

HRID 1451162 반응식
Cl[C:2]([C:16]1[N:21]=[C:20]([O:22][CH3:23])[CH:19]=[C:18]([O:24][CH3:25])[N:17]=1)([C:10]1[CH:15]=[CH:14][CH:13]=[CH:12][CH:11]=1)[C:3]([NH:5][S:6]([CH3:9])(=[O:8])=[O:7])=[O:4].[C:26]([O-:29])(=[O:28])[CH3:27].[Na+]>C(O)(=O)C>[C:26]([O:29][C:2]([C:16]1[N:21]=[C:20]([O:22][CH3:23])[CH:19]=[C:18]([O:24][CH3:25])[N:17]=1)([C:10]1[CH:15]=[CH:14][CH:13]=[CH:12][CH:11]=1)[C:3]([NH:5][S:6]([CH3:9])(=[O:8])=[O:7])=[O:4])(=[O:28])[CH3:27]

참가 물질

4

반응물 2

HCID 517045Sodium AcetateHCID 199739322-Chloro-2-(4,6-dimethoxypyrimidin-2-yl)-N-methanesulfonyl-2-phenylacetamide

생성물 1

HCID 677141702-Acetoxy-2-(4,6-dimethoxypyrimidin-2-yl)-N-methanesulfony-2-phenylacetamide수율 98%

시약·촉매·용매 1

HCID 176Acetic Acid용매

실험 절차

2-Chloro-2-(4,6-dimethoxypyrimidin-2-yl)-N-methanesulfonyl-2-phenylacetamide (0.5 g) and anhydrous sodium acetate (0.25 g) were refluxed in glacial acetic acid (10 ml) for 7 hours. The acetic acid was evaporated off under vacuum, and the residue was taken into ether. The ether solution was washed with water (3 times), dried over magnesium sulfate, and evaporated under vacuum to give 0.52 g of a brown glass. Trituration with diisopropyl ether gave an off-white solid, which was filtered off, washed with diisopropyl ether and dried to give 0.3 g of the desired product, mp 141°-143° C.

후처리

  1. customThe acetic acid was evaporated off under vacuum
  2. washThe ether solution was washed with water (3 times)
  3. dry with materialdried over magnesium sulfate
  4. customevaporated under vacuum

출처 및 근거

ORD 기록
ord-5db6ada7970a4ff68736fef82eeba95f
출처 데이터셋
uspto-grants-1997_02
특허 번호
US05604181

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