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Water → (R)-2-methyl-propane-2-sulfinic acid [(S)-1-(4-bromo-2-methyl-phenyl)-ethyl]amide

HRID 1640855
ノート
印刷プレビュー

反応式

HRID 1640855 の反応式
C([BH-](C(CC)C)C(CC)C)(CC)C.[Li+].[Br:15][C:16]1[CH:21]=[CH:20][C:19]([C:22](=[N:24][S@@:25]([C:27]([CH3:30])([CH3:29])[CH3:28])=[O:26])[CH3:23])=[C:18]([CH3:31])[CH:17]=1.O>O1CCCC1>[Br:15][C:16]1[CH:21]=[CH:20][C:19]([C@@H:22]([NH:24][S@@:25]([C:27]([CH3:30])([CH3:29])[CH3:28])=[O:26])[CH3:23])=[C:18]([CH3:31])[CH:17]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 962WaterHCID 3611392Lithium tri-s-butylborohydrideHCID 86649414(R)-2-Methyl-propane-2-sulfinic acid [1-(4-bromo-2-methyl-phenyl)-ethylidene]-amide

生成物 1

HCID 58102376(R)-2-methyl-propane-2-sulfinic acid [(S)-1-(4-bromo-2-methyl-phenyl)-ethyl]amide

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

Lithium tri-sec-butylborohydride (1 mol/L in tetrahydrofuran, 59.2 mL) was added to a solution of (R)-2-methyl-propane-2-sulfinic acid [1-(4-bromo-2-methyl-phenyl)-ethylidene]-amide (6.24 g) in tetrahydrofuran (50 mL) chilled in an ice bath. The solution was stirred for 2 h while warming to room temperature in the cooling bath. The solution was then cooled again in an ice bath prior to the careful addition of water. The resulting mixture was extracted with ethyl acetate and the combined extracts were washed with water, saturated aqueous NaHCO3 solution, and brine. After drying (MgSO4) and evaporating the solvent, the title compound was obtained that was directly submitted to the next reaction step. Yield: 8.85 g (ca. 75% pure); Mass spectrum (ESI−): m/z=318/320 (Br) [M+H]+.

後処理

  1. temperaturechilled in an ice bath
  2. temperatureThe solution was then cooled again in an ice bath
  3. extractionThe resulting mixture was extracted with ethyl acetate
  4. washthe combined extracts were washed with water, saturated aqueous NaHCO3 solution, and brine
  5. dry with materialAfter drying (MgSO4)
  6. customevaporating the solvent

出典と根拠

ORDレコード
ord-6c781cc29605483386af1e47b643ecb6
出典データセット
uspto-grants-2012_02
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08114868B2

反応ノート

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