Carbon Tetrachloride → HCID 66790033, compound

HRID 1510120Notes

Reaction equation

HRID 1510120 reaction equation
[F:1][C:2]1[CH:7]=[CH:6][C:5]([O:8][C@H:9]([CH3:12])[CH2:10][CH3:11])=[CH:4][C:3]=1[CH2:13]O.C1C=CC(P(C2C=CC=CC=2)C2C=CC=CC=2)=CC=1.C(Cl)(Cl)(Cl)[Cl:35]>>[Cl:35][CH2:13][C:3]1[CH:4]=[C:5]([O:8][C@H:9]([CH3:12])[CH2:10][CH3:11])[CH:6]=[CH:7][C:2]=1[F:1]

Participants

4

Reactant 3

HCID 5943Carbon TetrachlorideHCID 11776TriphenylphosphineHCID 66790401HCID 66790401, compound

Product 1

HCID 66790033HCID 66790033, compound

Conditions

Temperature
78 °C

Procedure

To a solution of (2-fluoro-5-{[(1R)-1-methylpropyl]oxy}phenyl)methanol (0.091 g, 0.459 mmol) in carbon tetrachloride (4.59 ml) was added triphenylphosphine resin (0.241 g, 0.918 mmol). The reaction was heated to 78° C. overnight in a pressure tube with minimal stirring. The reaction mixture was filtered through a fritted funnel and washed with carbon tetrachloride. The filtrate was concentrated to give the desired product.

Workup

  1. filtrationThe reaction mixture was filtered through a fritted funnel
  2. washwashed with carbon tetrachloride
  3. concentrationThe filtrate was concentrated

Sources & evidence

ORD record
ord-5749d43211d24ebebfff225ea1e6d748
Source dataset
uspto-grants-2012_07
Patent number
US08211904B2

Reaction notes

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