Trifluoroacetic anhydride → HCID 54333950、化合物

HRID 2301032ノート

反応式

HRID 2301032 の反応式
FC(F)(F)C(OC(=O)C(F)(F)F)=O.[Cl:14][C:15]1[CH:20]=[C:19]([S:21](C)=O)[CH:18]=[CH:17][C:16]=1[NH:24][C:25](=[O:33])[C@:26]([OH:32])([CH3:31])[C:27]([F:30])([F:29])[F:28]>>[Cl:14][C:15]1[CH:20]=[C:19]([SH:21])[CH:18]=[CH:17][C:16]=1[NH:24][C:25](=[O:33])[C@:26]([OH:32])([CH3:31])[C:27]([F:30])([F:28])[F:29]

参加物

3

反応物 2

HCID 9845Trifluoroacetic anhydrideHCID 69113436HCID 69113436、化合物

生成物 1

HCID 54333950HCID 54333950、化合物収率 103.6%

実験手順

Trifluoroacetic anhydride (5 ml) was added to (R)-N-(2-chloro-4-methylsulphinyl-phenyl)-2-hydroxy-2-methyl-3,3,3-trifluoropropanamide (Example 92) (0.188 g). The mixture was stirred and heated under reflux for 45 minutes then cooled and evaporated to dryness. A mixture of triethylamine (5 ml) and methanol (5 ml) was added to the residue. This mixture was stirred for a further 45 minutes then evaporated to dryness. The residue was dissolved in chloroform (50 ml), washed with saturated aqueous ammonium chloride solution (50 ml), dried and concentrated by evaporation to give the title compound (0.177 g) as a gum which was used without purification. MS (ESP−): 298.

後処理

  1. temperatureheated
  2. temperatureunder reflux for 45 minutes
  3. temperaturethen cooled
  4. customevaporated to dryness
  5. additionA mixture of triethylamine (5 ml) and methanol (5 ml)
  6. additionwas added to the residue
  7. stirringThis mixture was stirred for a further 45 minutes
  8. customthen evaporated to dryness
  9. dissolutionThe residue was dissolved in chloroform (50 ml)
  10. washwashed with saturated aqueous ammonium chloride solution (50 ml)
  11. customdried
  12. concentrationconcentrated by evaporation

出典と根拠

ORDレコード
ord-0d2a27b884064e1d87d0556f83c549b7
出典データセット
uspto-grants-2002_12
特許番号
US06498275B1

反応ノート

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