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

HRID 1451160
ノート
印刷プレビュー

反応式

HRID 1451160 の反応式
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
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-03d39270d741449ab7d1b821e5d63e23
出典データセット
uspto-grants-1997_02
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05604181

反応ノート

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