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1-(3-Chlorophenyl)ethanone → (R)-1-(3-Chlorophenyl)ethanol

HRID 2177006
Notes
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Reaction equation

HRID 2177006 reaction equation
B.O1CCCC1.[CH3:7][C:8]([C:10]1[CH:15]=[CH:14][CH:13]=[C:12]([Cl:16])[CH:11]=1)=[O:9]>C1(C)C=CC=CC=1.O1CCCC1>[Cl:16][C:12]1[CH:11]=[C:10]([C@H:8]([OH:9])[CH3:7])[CH:15]=[CH:14][CH:13]=1
ParticipantsProcedureWorkupSources & evidenceReaction notes

Participants

5

Reactant 2

HCID 149331-(3-Chlorophenyl)ethanoneHCID 2723981Borane;tetrahydrofuran2×

Product 1

HCID 6950742(R)-1-(3-Chlorophenyl)ethanolYield 78%

Reagents, catalysts & solvents 2

HCID 1140TolueneSolventHCID 8028TetrahydrofuranSolvent

Procedure

To a solution of borane-tetrahydrofuran (0.647 mL, 0.647 mmol, Aldrich, 1 M solution in THF) and (S)-MeCBS (0.647 mL, 0.647 mmol, Aldrich, 1M solution in toluene) was added simultaneously a solution of 3-chloroacetophenone (1.00 g, 6.47 mmol) in anhydrous tetrahydrofuran (2.42 mL) and a solution of borane-tetrahydrofuran (3.24 mL, 3.24 mmol, Aldrich, 1 M solution in THF) over 30 min at ambient temperature. After complete addition, the reaction mixture was stirred for 10 min, quenched slowly at 0° C. with methanol (0.94 mL) and then saturated HCl in ether (0.12 mL). After stirring at 0° C. for 5 min and ambient temperature for 30 min, the solution was concentrated in vacuo to an oil. The oil was twice diluted with benzene and concentrated in vacuo, diluted with ether, and concentrated in vacuo to an oil. The oil was purified by flash chromatography(silica gel, 20% EA in hexane) to give (R)-1-(3-chlorophenyl)ethanol as a clear colorless oil (0.784 g, 78%). Optical rotation in CHCl3 at 20° C. at concentration 0.220 was +40.9° (Literature, Bull. Chem. Soc. Jpn. 1996, 69(4), 1079-1085, optical rotation in CHCl3 at 21° C. at concentration 0.220 was +44°).

Workup

  1. additionAfter complete addition
  2. customquenched slowly at 0° C. with methanol (0.94 mL)
  3. stirringAfter stirring at 0° C. for 5 min and ambient temperature for 30 min
  4. concentrationthe solution was concentrated in vacuo to an oil
  5. additionThe oil was twice diluted with benzene
  6. concentrationconcentrated in vacuo
  7. additiondiluted with ether
  8. concentrationconcentrated in vacuo to an oil
  9. customThe oil was purified by flash chromatography(silica gel, 20% EA in hexane)

Sources & evidence

ORD record
ord-cd0c8f07bb3e4858818e7dd63a01ae17
Source dataset
uspto-grants-2015_06
DOI
10.6084/m9.figshare.5104873.v1
Patent number
US09067897B2

Reaction notes

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On this pageParticipantsProcedureWorkupSources & evidenceReaction notes