Acetic Acid → HCID 16764602、化合物

HRID 2206844ノート

反応式

HRID 2206844 の反応式
[Cl:1][C:2]1[C:3]([C:10]([NH2:12])=[O:11])=[N:4][C:5](SC)=[N:6][CH:7]=1.[S:13]([O-:18])(O[O-])(=O)=[O:14].[K+].[K+].[C:21](O)(=O)C.CO>O>[Cl:1][C:2]1[C:3]([C:10]([NH2:12])=[O:11])=[N:4][C:5]([S:13]([CH3:21])(=[O:18])=[O:14])=[N:6][CH:7]=1

参加物

6

反応物 4

HCID 176Acetic AcidHCID 887MethanolHCID 10313463Potassium peroxymonosulphateHCID 16426513HCID 16426513、化合物

生成物 1

HCID 16764602HCID 16764602、化合物収率 17%

試薬・触媒・溶媒 1

HCID 962Water溶媒2 回

実験手順

7.7 g (37.8 mmo) of 5-chloro-2-(methylsulfanyl)pyrimidine-4-carboxamide and 37.2 g (60.4 mmol) of potassium peroxomonosulfate are suspended in a mixture of 30 ml of water, 30 ml of acetic acid and 30 ml of methanol, and the mixture is stirred for about 3 hours. The mixture is then taken up in about 100 ml of water and extracted with ethyl acetate. Drying and concentrating of the ethyl acetate extract gave 1.5 g of 5-chloro-2-(methylsulfonyl)pyrimidine-4-carboxamide (melting point 205° C., 17% yield at a purity of 95%). More 5-chloro-2-(methylsulfonyl)pyrimidine-4-carboxamide was able to be isolated from the mother liquor.

後処理

  1. extractionextracted with ethyl acetate
  2. customDrying
  3. concentrationconcentrating of the ethyl acetate
  4. extractionextract

出典と根拠

ORDレコード
ord-6a43298467b7452a91cf875679d67a2a
出典データセット
uspto-grants-2016_06
特許番号
US09375002B2

反応ノート

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