Methanol → Methyl 4,4,4-trifluoro-2-hydroxybutanoate

HRID 1486763ノート

反応式

HRID 1486763 の反応式
S(Cl)(Cl)=O.[F:5][C:6]([F:14])([F:13])[CH2:7][CH:8]([OH:12])[C:9]([OH:11])=[O:10].[CH3:15]O>>[F:5][C:6]([F:14])([F:13])[CH2:7][CH:8]([OH:12])[C:9]([O:11][CH3:15])=[O:10]

参加物

4

反応物 3

HCID 887MethanolHCID 24386Thionyl ChlorideHCID 198006174,4,4-Trifluoro-2-hydroxybutanoic acid

生成物 1

HCID 21600538Methyl 4,4,4-trifluoro-2-hydroxybutanoate

反応条件

温度
70 °C

実験手順

Thionyl chloride (0.139 ml, 1.90 mmol) was added dropwise to a solution of 12-2 (200 mg, 1.27 mmol) in MeOH (2 ml) at room temperature. After addition was complete, the reaction was heated in a sealed vessel at 70° C. for 2 h. The reaction was cooled to room temperature and concentrated in vacuo. The residue was diluted with 7N NH3/MeOH (3 mL) and filtered to remove insolubles. The filtrate was concentrated to dryness to afford 12-3 as a clear oil.

後処理

  1. additionAfter addition
  2. temperatureThe reaction was cooled to room temperature
  3. concentrationconcentrated in vacuo
  4. additionThe residue was diluted with 7N NH3/MeOH (3 mL)
  5. filtrationfiltered
  6. customto remove insolubles
  7. concentrationThe filtrate was concentrated to dryness

出典と根拠

ORDレコード
ord-19cf1507efbc4fac9d15401883d302ed
出典データセット
uspto-grants-2016_08
特許番号
US09428492B2

反応ノート

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