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

HRID 1451162ノート

反応式

HRID 1451162 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: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]

参加物

4

反応物 2

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 176Acetic Acid溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-5db6ada7970a4ff68736fef82eeba95f
出典データセット
uspto-grants-1997_02
特許番号
US05604181

反応ノート

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