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Ethanethiol → 3-Methoxy-4-(methylsulfanyl)phenol

HRID 1246624
Notes
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Reaction equation

HRID 1246624 reaction equation
[CH2:1]([O:8]CC1C=CC=CC=1)[C:2]1C=CC=[CH:4][CH:3]=1.[CH2:16]([SH:18])C.B(F)(F)F.C[CH2:24][O:25][CH2:26][CH3:27]>C(Cl)Cl>[CH3:24][O:25][C:26]1[CH:27]=[C:1]([OH:8])[CH:2]=[CH:3][C:4]=1[S:18][CH3:16]
ParticipantsProcedureWorkupSources & evidenceReaction notes

Participants

5

Reactant 3

HCID 6343EthanethiolHCID 7657Dibenzyl etherHCID 8000Boron trifluoride etherate

Product 1

HCID 218771303-Methoxy-4-(methylsulfanyl)phenolYield 28%

Reagents, catalysts & solvents 1

HCID 6344DichloromethaneSolvent

Procedure

The benzylether from stage (iii) (9.27 g, 39.5 mmol) was dissolved in DCM (5 mL), ethanethiol (5 mL) and BF3.OEt2 (5 mL, 39.5 mol) were then added at room temperature under a nitrogen atmosphere. The mixture was stirred overnight before the reaction was quenched with 2M HCl and stirred for a further 30 min. The mixture was then basified by the addition of 2M NaOH until pH 10 was attained. The mixture was then washed with EtOAc (3×50 mL). The aqueous layer was re-acidified by the addition of 2M HCl to pH 1 and extracted with EtOAc (4×50 mL). The extracts were combined, dried (MgSO4) and evaporated to an oil. Purification by flash chromatography [SiO2; EtOAc/pentane (1:9→1:4)] afforded the desired phenol compound as a colourless solid (1.73 g, 28%); δH (CDCl3, 400 MHz) 2.21 (3H, s), 3.70 (3H, s), 6.30 (1H, d), 6.35 (1H, s), 6.96 (1H, d), 9.39 (1H, brs).

Workup

  1. customwas quenched with 2M HCl
  2. stirringstirred for a further 30 min
  3. additionThe mixture was then basified by the addition of 2M NaOH until pH 10
  4. washThe mixture was then washed with EtOAc (3×50 mL)
  5. additionThe aqueous layer was re-acidified by the addition of 2M HCl to pH 1
  6. extractionextracted with EtOAc (4×50 mL)
  7. dry with materialdried (MgSO4)
  8. customevaporated to an oil
  9. customPurification by flash chromatography [SiO2; EtOAc/pentane (1:9→1:4)]

Sources & evidence

ORD record
ord-06e630104681478e9148516800170974
Source dataset
uspto-grants-2006_10
DOI
10.6084/m9.figshare.5104873.v1
Patent number
US07129234B2

Reaction notes

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On this pageParticipantsProcedureWorkupSources & evidenceReaction notes