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Propargyl bromide → 4-Difluoromethyl-4-hydroxy-1-octyne

HRID 848904
Notes
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Reaction equation

HRID 848904 reaction equation
[Mg].[CH2:2](Br)[C:3]#[CH:4].[F:6][CH:7]([F:14])[C:8](=[O:13])[CH2:9][CH2:10][CH2:11][CH3:12]>CCOCC>[F:6][CH:7]([F:14])[C:8]([OH:13])([CH2:9][CH2:10][CH2:11][CH3:12])[CH2:4][C:3]#[CH:2]
ParticipantsProcedureWorkupSources & evidenceReaction notes

Participants

5

Reactant 3

HCID 7842Propargyl bromide2×HCID 5462224MagnesiumHCID 217647851,1-Difluoro-2-hexanone

Product 1

HCID 127861894-Difluoromethyl-4-hydroxy-1-octyne

Reagents, catalysts & solvents 1

HCID 3283Diethyl EtherSolvent2×

Procedure

To a stirred suspension of 3.6 g. of magnesium and 30 mg. of mercuric chloride in 0.33 ml. of ether is added 1.5 ml. of propargyl bromide. The mixture is stirred vigorously for several minutes to initiate reaction, then a solution of 15.5 g. of 1,1-difluoro-2-hexanone and 12.1 ml. of propargyl bromide in 33 ml. of ether is added slowly (dropwise) over a 1.5 hour period, so that the mixture remains gently refluxing (25°-30° C.). After addition, the mixture is stirred at room temperature for 30 minutes, then cooled in an ice bath to 0°-5° C. and quenched by adding 35 ml. of saturated ammonium chloride solution dropwise and then stirred for 30 minutes. The mixture is filtered through Celite and washed with ether. The filtrate is concentrated in vacuo giving a yellow oil. This oil is vacuum distilled at 71° C., 12 mm giving the product as 10.54 g. of colorless oil which becomes pale yellow on standing at room temperature.

Workup

  1. additionTo a stirred suspension of 3.6 g
  2. customreaction
  3. temperatureso that the mixture remains gently refluxing (25°-30° C.)
  4. additionAfter addition
  5. stirringthe mixture is stirred at room temperature for 30 minutes
  6. temperaturecooled in an ice bath to 0°-5° C.
  7. customquenched
  8. additionby adding 35 ml
  9. stirringof saturated ammonium chloride solution dropwise and then stirred for 30 minutes
  10. filtrationThe mixture is filtered through Celite
  11. washwashed with ether
  12. concentrationThe filtrate is concentrated in vacuo
  13. customgiving a yellow oil
  14. distillationdistilled at 71° C.
  15. custom12 mm giving the product as 10.54 g
  16. customon standing at room temperature

Sources & evidence

ORD record
ord-66596a0b9f494f59aa0c50c14313dc4c
Source dataset
uspto-grants-1981_10
DOI
10.6084/m9.figshare.5104873.v1
Patent number
US04297516

Reaction notes

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On this pageParticipantsProcedureWorkupSources & evidenceReaction notes