Sodium Sulfate → HCID 18006318, compound

HRID 989477Notes

Reaction equation

HRID 989477 reaction equation
Cl[B:2]([CH:14]1[CH2:18][CH2:17][CH2:16][CH:15]1[C:19]1[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=1)[CH:3]1[CH2:7][CH2:6][CH2:5][CH:4]1[C:8]1[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=1.[CH3:25][Al](C)C.[Cl-].[NH4+].S([O-])([O-])(=O)=O.[Na+].[Na+]>CCCCCC>[CH3:25][B:2]([CH:14]1[CH2:18][CH2:17][CH2:16][CH:15]1[C:19]1[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=1)[CH:3]1[CH2:7][CH2:6][CH2:5][CH:4]1[C:8]1[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=1

Participants

6

Reactant 4

HCID 24436Sodium SulfateHCID 25517Ammonium ChlorideHCID 16682925TrimethylaluminumHCID 18006355HCID 18006355, compound

Product 1

HCID 18006318HCID 18006318, compound

Reagents, catalysts & solvents 1

HCID 8058HexaneSolvent

Conditions

Temperature
0 °C

Procedure

Chloro-bis-(2-phenyl-cyclopentyl)-borane from preparation 1 was diluted with 60 mL of dry hexanes under nitrogen. The solution was cooled to 0° C. and a 2M solution of trimethylaluminum in hexanes (5.8 mL) was added dropwise causing the reaction to turn orange. The reaction was allowed to warm to room temperature and stirred for 1.5 hours. During this time a red-brown mass precipitated out of solution, leaving a yellow supernatant. The hexane supernatant was transferred via cannula to a nitrogen flushed separatory funnel containing 50 mL of saturated aqueous ammonium chloride. The organic phase becomes colorless and was transferred via cannula to a dry flask containing sodium sulfate for drying. The solution was then transferred via cannula to a dry, nitrogen-flushed flask and the solvent removed under aspirator vacuum and nitrogen. The clear oil was used directly without further characterization.

Workup

  1. customthe reaction
  2. temperatureto warm to room temperature
  3. customDuring this time a red-brown mass precipitated out of solution
  4. customleaving a yellow supernatant
  5. customwas transferred via cannula to a dry flask
  6. customfor drying
  7. customflushed flask
  8. customthe solvent removed under aspirator vacuum and nitrogen

Sources & evidence

ORD record
ord-138666e3676945c488a9dcef9c750ec1
Source dataset
uspto-grants-2003_10
Patent number
US06639107B1

Reaction notes

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