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Potassium Bicarbonate → 2-(4,6-Dimethoxypyrimidin-2-yl)-2-hydroxy N-methanesulfonyl-2-phenylacetamide

HRID 1451160
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HRID 1451160 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(=O)(O)[O-:27].[K+]>O>[CH3:25][O:24][C:18]1[CH:19]=[C:20]([O:22][CH3:23])[N:21]=[C:16]([C:2]([OH:27])([C:10]2[CH:15]=[CH:14][CH:13]=[CH:12][CH:11]=2)[C:3]([NH:5][S:6]([CH3:9])(=[O:8])=[O:7])=[O:4])[N:17]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 516893Potassium BicarbonateHCID 199739322-Chloro-2-(4,6-dimethoxypyrimidin-2-yl)-N-methanesulfonyl-2-phenylacetamide

생성물 1

HCID 199739352-(4,6-Dimethoxypyrimidin-2-yl)-2-hydroxy N-methanesulfonyl-2-phenylacetamide수율 94.5%

시약·촉매·용매 1

HCID 962Water용매

실험 절차

2-Chloro-2-(4,6-dimethoxypyrimidin-2-yl)-N-methanesulfonyl-2-phenylacetamide (0.5 g) was stirred at room temperature with potassium bicarbonate (0.2 g) in water (10 ml) for 2 hours, by which time all was in solution. After standing for 3 days, the solution was washed with ether (twice) and acidified with hydrochloric acid. Ether extraction (3 times), washing with water (twice), drying over magnesium sulfate and evaporation under vacuum gave 0.45 g of the desired product as a yellow glass. This glass slowly crystallised to a solid, mp 94°-6° C.

후처리

  1. washthe solution was washed with ether (twice) and
  2. extractionEther extraction (3 times)
  3. washwashing with water (twice),
  4. dry with materialdrying over magnesium sulfate and evaporation under vacuum

출처 및 근거

ORD 기록
ord-03d39270d741449ab7d1b821e5d63e23
출처 데이터셋
uspto-grants-1997_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05604181

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