Iodine → HCID 178506003, compound

HRID 1963252Notes

Reaction equation

HRID 1963252 reaction equation
[Zn:1].II.[Br:4][CH2:5][CH:6]1[CH2:11][CH2:10][C:9]([F:13])([F:12])[CH2:8][CH2:7]1>CC(N(C)C)=O>[Br-:4].[F:12][C:9]1([F:13])[CH2:10][CH2:11][CH:6]([CH2:5][Zn+:1])[CH2:7][CH2:8]1

Participants

5

Reactant 3

HCID 807IodineHCID 23994ZincHCID 533503614-(Bromomethyl)-1,1-difluorocyclohexane

Product 1

HCID 178506003HCID 178506003, compound

Reagents, catalysts & solvents 1

HCID 31374DimethylacetamideSolvent

Conditions

Temperature
70 °C

Procedure

Zinc powder (1.43 g, 21.87 mmol) was added to a dried flask and was heated at 70° C. under vacuum for 30 minutes. Dry DMA (29 mL) and iodine (0.092 g, 0.37 mmol) were added and the mixture was heated at 70° C. until the red-brown colour had disappeared (approx. 5 minutes). 4-(Bromomethyl)-1,1-difluorocyclohexane (3.1 g, 14.55 mmol) was added and heating was continued for ca. 42 h. The resulting solution was used in the next transformation.

Workup

  1. temperaturethe mixture was heated at 70° C. until the red-brown colour
  2. custom(approx. 5 minutes)
  3. temperatureheating

Sources & evidence

ORD record
ord-515558435e7646caacaf978344a2cf2a
Source dataset
uspto-grants-2013_04
Patent number
US08415378B2

Reaction notes

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