Trifluoroacetic anhydride → HCID 54333950, 화합물

HRID 841199노트

반응식

HRID 841199 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-methylsulphinylphenyl)-2-hydroxy-2-methyl-3,3,3-trifluoropropanamide (Method 32)(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 298 (M−H)−.

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-779623b53fb54f1582e7d07346b8aa88
출처 데이터셋
uspto-grants-2002_04
특허 번호
US06369273B1

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