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Chlorotrimethylsilane → 2-Amino-4,4,4-trifluorobutan-1-ol

HRID 1594326
ノート
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反応式

HRID 1594326 の反応式
C[Si](Cl)(C)C.[BH4-].[Li+].[NH2:8][CH:9]([CH2:13][C:14]([F:17])([F:16])[F:15])[C:10](O)=[O:11]>C1COCC1>[NH2:8][CH:9]([CH2:13][C:14]([F:17])([F:16])[F:15])[CH2:10][OH:11]
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 6397ChlorotrimethylsilaneHCID 3530832-Amino-4,4,4-trifluorobutanoic acidHCID 4148881Lithium borohydride

生成物 1

HCID 534164332-Amino-4,4,4-trifluorobutan-1-ol収率 38.2%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

A solution of trimethylsilyl chloride (1.38 g, 12.73 mmol) was added to a solution of lithium borohydride (3.2 mL, 2.0 M in THF) and THF (5 mL) at 25° C. After stirring 5 min, 2-amino-4,4,4-trifluoro-butyric acid (0.50 g, 3.18 mmol) was added portionwise over a 5 min period. The reaction was allowed to stir 48 h. The reaction was quenched by cautious addition of MeOH (5 mL) dropwise. The solvent was evaporated and the residue treated with potassium hydroxide (KOH) solution (20%, 6 mL). The aqueous phase was extracted using dichloromethane, 3 times (10 mL each). The organic phases were combined and dried over anhydrous sodium sulfate. After filtration the solvent was evaporated to afford the 2-amino-4,4,4-trifluoro-butan-1-ol as an oil (0.174 g, 38%). This oil was used directly in the next reaction without further purification.

後処理

  1. stirringto stir 48 h
  2. customThe reaction was quenched by cautious addition of MeOH (5 mL) dropwise
  3. customThe solvent was evaporated
  4. additionthe residue treated with potassium hydroxide (KOH) solution (20%, 6 mL)
  5. extractionThe aqueous phase was extracted
  6. dry with materialdried over anhydrous sodium sulfate
  7. filtrationAfter filtration the solvent
  8. customwas evaporated

出典と根拠

ORDレコード
ord-1c8f2c67c3b84ec5a07f8af0d6f4bfc4
出典データセット
uspto-grants-2007_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07300951B2

反応ノート

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