Trifluoroacetic anhydride → HCID 54333950, 화합물

HRID 1062374노트

반응식

HRID 1062374 반응식
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]

참가 물질

3

반응물 2

HCID 9845Trifluoroacetic anhydrideHCID 69113436HCID 69113436, 화합물

생성물 1

HCID 54333950HCID 54333950, 화합물수율 103.6%

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-1c83908a03e24c73a98e627940cd2f42
출처 데이터셋
uspto-grants-2005_11
특허 번호
US06960688B2

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