Methanol → Methyl 4-amino-2-(methylsulfonyl)thiazole-5-carboxylate

HRID 1161514ノート

反応式

HRID 1161514 の反応式
[CH3:1][O:2][C:3]([C:5]1[S:9][C:8](SC)=[N:7][C:6]=1[NH2:12])=[O:4].[CH3:13]O.O[O:16][S:17]([O-:19])=O.[K+]>O.C(OCC)(=O)C>[CH3:1][O:2][C:3]([C:5]1[S:9][C:8]([S:17]([CH3:13])(=[O:19])=[O:16])=[N:7][C:6]=1[NH2:12])=[O:4]

参加物

6

反応物 3

HCID 887MethanolHCID 609212Methyl 4-amino-2-(methylsulfanyl)-1,3-thiazole-5-carboxylateHCID 23707502Potassium hydroxy sulfite

生成物 1

HCID 59511825Methyl 4-amino-2-(methylsulfonyl)thiazole-5-carboxylate

試薬・触媒・溶媒 2

HCID 962Water溶媒2 回HCID 8857Ethyl Acetate溶媒

実験手順

After adding 45.2 g of 4-amino-2-methylsulfanylthiazole-5-carboxylic acid methyl ester [CAS No. 60093-05-2] to 2 liters of a water:methanol=1:1 mixed solvent at room temperature, 408 g of Oxone was added in small portions over a period of 30 minutes with stirring. The mixture was stirred at room temperature for 24 hours, and then poured into a mixture of 10 liters of ethyl acetate and 10 liters of water. After washing the organic layer with 5 liters of saturated brine, it was dried over anhydrous magnesium sulfate. The desiccating agent was filtered off, and the filtrate was concentrated under reduced pressure to give the title compound (37.6 g) as a white solid.

後処理

  1. stirringThe mixture was stirred at room temperature for 24 hours
  2. washAfter washing the organic layer with 5 liters of saturated brine, it
  3. dry with materialwas dried over anhydrous magnesium sulfate
  4. filtrationThe desiccating agent was filtered off
  5. concentrationthe filtrate was concentrated under reduced pressure

出典と根拠

ORDレコード
ord-f8868a0534fa4200ad72ce3db3b9ac99
出典データセット
uspto-grants-2010_10
特許番号
US07816522B2

反応ノート

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