Sodium Thiosulfate → (R)-2-Methyl-4,4,4-trifluorobutanal
反応式
[F:1][C:2]([F:9])([F:8])[CH2:3][C@@H:4]([CH3:7])[CH2:5][OH:6].CC(OI1(OC(C)=O)(OC(C)=O)OC(=O)C2C=CC=CC1=2)=O.[O-]S([O-])(=S)=O.[Na+].[Na+]>C(Cl)Cl.C(OCC)C.C([O-])(O)=O.[Na+]>[F:1][C:2]([F:9])([F:8])[CH2:3][C@@H:4]([CH3:7])[CH:5]=[O:6]参加物
7
反応条件
- 温度
- 25 °C
実験手順
To (2R)-4,4,4-trifluoro-2-methylbutan-1-ol (2.90 g, 20.4 mmol) in CH2Cl2 (50 mL) at 0° C. was added Dess-Martin periodinane (10.24 g, 24.49 mmol). After 15 min, the reaction mixture was warmed to 25° C. and stirred for 1 h. This mixture was then diluted with diethyl ether (50 mL) and added to Na2S2O3 (11.29 g, 71.44 mmol) dissolved in a saturated solution of aqueous NaHCO3 (100 mL). The milky white mixture was stirred until both layers were homogeneous. The phases were separated and the organic extract was dried (MgSO4) and filtered to give a solution of (2R)-4,4,4-trifluoro-2-methylbutanal which was used in the next step without removal of solvents.
後処理
- stirringThe milky white mixture was stirred until both layers
- customThe phases were separated
- extractionthe organic extract
- dry with materialwas dried (MgSO4)
- filtrationfiltered
出典と根拠
- ORDレコード
- ord-157d631fcbd340cba8fe07c51fa7bca7
- 出典データセット
- uspto-grants-2007_11
- 特許番号
- US07300951B2
反応ノート
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