Isopropanol → HCID 86619918, compound

HRID 1970723Notes

Reaction equation

HRID 1970723 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 0 C 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 0 C 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-533e62fdb41349b9a24882e135f7b429
Source dataset
uspto-grants-2013_04
Patent number
US08431045B2

Reaction notes

Loading…