Isopropanol → HCID 86619918, compound

HRID 1471270Notes

Reaction equation

HRID 1471270 reaction equation
CC(O)C.[CH2:5]([P:9]([CH2:12][CH:13]([CH3:15])[CH3:14])(=[S:11])[SH:10])[CH:6]([CH3:8])[CH3:7].[OH-].[CH2:17]([N+:21]([CH2:30][CH2:31][CH2:32][CH3:33])([CH2:26][CH2:27][CH2:28][CH3:29])[CH2:22][CH2:23][CH2:24][CH3:25])[CH2:18][CH2:19][CH3:20].CCCCCC>O>[CH2:5]([P:9]([CH2:12][CH:13]([CH3:15])[CH3:14])(=[S:10])[S-:11])[CH:6]([CH3:8])[CH3:7].[CH2:30]([N+:21]([CH2:17][CH2:18][CH2:19][CH3:20])([CH2:22][CH2:23][CH2:24][CH3:25])[CH2:26][CH2:27][CH2:28][CH3:29])[CH2:31][CH2:32][CH3:33]

Participants

6

Reactant 4

HCID 3776IsopropanolHCID 8058HexaneHCID 83376Bis(2-methylpropyl)phosphinodithioic acidHCID 2723671Tetrabutylammonium Hydroxide

Product 1

HCID 86619918HCID 86619918, compound

Reagents, catalysts & solvents 1

HCID 962WaterSolvent

Procedure

To 40 ml of 2-propanol, 3.63 g diisobutyldithiophosphinic acid and 7.34 g of 55-60% by weight tetrabutylammonium hydroxide in water were added. The mixture was stirred under nitrogen for one hour. The solvent was removed by distillation. To remove residual water, 2-propanol was twice added and subsequently removed by distillation. The liquid was cooled to less than OC for 16 hours. To the precipitates that formed, a small amount of hexane was added to give a slurry. The slurry was filtered, washed with hexane, and dried under reduced pressure yielding 6.07 g of a white solid.

Workup

  1. customThe solvent was removed by distillation
  2. customTo remove residual water, 2-propanol
  3. additionwas twice added
  4. customsubsequently removed by distillation
  5. temperatureThe liquid was cooled to less than OC for 16 hours
  6. customTo the precipitates
  7. customthat formed
  8. customto give a slurry
  9. filtrationThe slurry was filtered
  10. washwashed with hexane
  11. customdried under reduced pressure

Sources & evidence

ORD record
ord-f787547643924f67ad1368616d32a28c
Source dataset
uspto-grants-2015_04
Patent number
US09011734B2

Reaction notes

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