Hydroxylamine HCl → HCID 59115139、化合物

HRID 1358159ノート

反応式

HRID 1358159 の反応式
[F:1][C:2]([F:14])([F:13])[C:3]([C:5]1[CH:10]=[CH:9][C:8]([S:11][CH3:12])=[CH:7][CH:6]=1)=O.[Cl-].[OH:16][NH3+:17].C([O-])(=O)C.[Na+]>C(O)C.O>[F:1][C:2]([F:14])([F:13])[C:3]([C:5]1[CH:10]=[CH:9][C:8]([S:11][CH3:12])=[CH:7][CH:6]=1)=[N:17][OH:16]

参加物

6

反応物 3

HCID 21645Hydroxylamine HClHCID 517045Sodium AcetateHCID 27606164'-Thiomethyl-2,2,2-trifluoroacetophenone

生成物 1

HCID 59115139HCID 59115139、化合物収率 54%

試薬・触媒・溶媒 2

HCID 702Ethanol溶媒HCID 962Water溶媒

実験手順

49.3 g (224 mmol) of 2,2,2-trifluoro-1-(4-methylsulfanyl-phenyl)-ethanone are dissolved in 250 ml of hot ethanol. To this solution is added dropwise a solution of hydroxylammonium chloride (16.3 g, 235 mmol) and sodium acetate (31.2 g, 381 mmol) in 125 ml of water, and the reaction solution is stirred under reflux for 6.5 hr. The reaction mixture was concentrated by rotary evaporation and poured into ice/water. The resulting yellow solid is filterd and washed with water. After drying under reduced pressure, recrystallization from hexane-ethyl acetate affords 28.4 g of white solid (54%). The structure is confirmed by the 1H-NMR spectrum (CDCl3), δ[ppm]:: d 2.51 (s, 3H), 7.31 (d, 2H), 7.49 (d, 2H), 8.80 (broad s, 1H).

後処理

  1. temperatureunder reflux for 6.5 hr
  2. concentrationThe reaction mixture was concentrated by rotary evaporation
  3. additionpoured into ice/water
  4. washwashed with water
  5. dry with materialAfter drying under reduced pressure, recrystallization from hexane-ethyl acetate

出典と根拠

ORDレコード
ord-a16d994533da42cbab56bba4b6f2f8d7
出典データセット
uspto-grants-2003_07
特許番号
US06596445B1

反応ノート

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