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

HRID 1365550
Notes
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Reaction equation

HRID 1365550 reaction equation
[Li+].[BH4-].C[Si](Cl)(C)C.[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]
ParticipantsProcedureWorkupSources & evidenceReaction notes

Participants

5

Reactant 3

HCID 6397ChlorotrimethylsilaneHCID 3530832-Amino-4,4,4-trifluorobutanoic acidHCID 4148881Lithium borohydride

Product 1

HCID 534164332-Amino-4,4,4-trifluorobutan-1-olYield 53.4%

Reagents, catalysts & solvents 1

HCID 8028TetrahydrofuranSolvent

Procedure

To a suspension of LiBH4 (62.7 mg, 2.88 mmol) in THF (1.5 mL) was added TMSCl (728 μL, 5.76 mmol) and the reaction mixture was stirred at room temperature for 15 min, followed by the addition of 2-amino-4,4,4-trifluorobutanoic acid (226 mg, 1.44 mmol). The reaction mixture was stirred at room temperature for 18 h, and quenched by careful addition of MeOH. The solvents were removed by reduced pressure, and to the residue was added H2O (2.08 mL). The resulting aqueous portion was made basic by adding 2 N NaOH. The mixture was extracted with CH2Cl2 three times. The combined organic portions were dried over MgSO4, filtered and concentrated to give 2-amino-4,4,4-trifluorobutan-1-ol as a colorless oil (110 mg, 53% yield). NMR: 400 MHz 1H (CDCl3) 3.61 ppm, 1 H, dd, J=10.61, 4.04 Hz; 3.42 ppm, 1 H, m; 3.28 ppm, 1 H, m; 2.29 ppm, 1 H, m; 2.12 ppm, 1 H, m.

Workup

  1. stirringThe reaction mixture was stirred at room temperature for 18 h
  2. customquenched by careful addition of MeOH
  3. customThe solvents were removed by reduced pressure
  4. additionto the residue was added H2O (2.08 mL)
  5. additionby adding 2 N NaOH
  6. extractionThe mixture was extracted with CH2Cl2 three times
  7. dry with materialThe combined organic portions were dried over MgSO4
  8. filtrationfiltered
  9. concentrationconcentrated

Sources & evidence

ORD record
ord-401086c64e2c4d21b2e5e4d4ece259c1
Source dataset
uspto-grants-2011_02
DOI
10.6084/m9.figshare.5104873.v1
Patent number
US07888376B2

Reaction notes

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On this pageParticipantsProcedureWorkupSources & evidenceReaction notes