Trifluoroacetic acid → N-[4-[(4-Chlorophenyl)sulfonyl]-4-(2,5-difluorophenyl)-3-methylbutyl]methanesulfonamide

HRID 748788ノート

反応式

HRID 748788 の反応式
[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([S:8]([CH:11]([C:28]2[CH:33]=[C:32]([F:34])[CH:31]=[CH:30][C:29]=2[F:35])[CH:12]([CH3:27])[CH2:13][CH2:14][N:15]([S:23]([CH3:26])(=[O:25])=[O:24])C(=O)OC(C)(C)C)(=[O:10])=[O:9])=[CH:4][CH:3]=1.FC(F)(F)C(O)=O.C(OCC)(=O)C.CCCCCC>ClCCl>[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([S:8]([CH:11]([C:28]2[CH:33]=[C:32]([F:34])[CH:31]=[CH:30][C:29]=2[F:35])[CH:12]([CH3:27])[CH2:13][CH2:14][NH:15][S:23]([CH3:26])(=[O:25])=[O:24])(=[O:10])=[O:9])=[CH:4][CH:3]=1

参加物

5

反応物 3

HCID 6422Trifluoroacetic acidHCID 21226206Ethyl acetate hexaneHCID 59750918t-Butyl N-[4-[(4-chlorophenyl)sulfonyl]-4-(2,5-difluorophenyl)-3-methylbutyl]-N-methylsulfonylcarbamate

生成物 1

HCID 9955499N-[4-[(4-Chlorophenyl)sulfonyl]-4-(2,5-difluorophenyl)-3-methylbutyl]methanesulfonamide収率 89.4%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒2 回

実験手順

The t-butyl N-[4-[(4-chlorophenyl)sulfonyl]-4-(2,5-difluorophenyl)-3-methylbutyl]-N-methylsulfonylcarbamate (136 mg, 0.246 mmol) obtained in Example 243 was dissolved in dichloromethane (4 ml), followed by the addition of trifluoroacetic acid (1 ml) at room temperature. After stirring at room temperature for 6 hours, the reaction mixture was diluted with dichloromethane, washed successively with water, a saturated aqueous solution of sodium bicarbonate, and brine, dried over magnesium sulfate and then, concentrated. The solid thus obtained was recrystallized from ethyl acetate-hexane, whereby the title compound (99.5 mg, 0.220 mmol, 89%) was obtained as colorless needle crystals.

後処理

  1. washwashed successively with water
  2. dry with materiala saturated aqueous solution of sodium bicarbonate, and brine, dried over magnesium sulfate
  3. concentrationconcentrated
  4. customThe solid thus obtained

出典と根拠

ORDレコード
ord-922e92dd585e428c9a799fe5e27e1b0b
出典データセット
uspto-grants-2008_07
特許番号
US07399775B2

反応ノート

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