Hydrochloric Acid → HCID 11982347, compound

HRID 343541Notes

Reaction equation

HRID 343541 reaction equation
[O:1]1CCCC1.[C:6]1([Si:12]2([C:42]3[CH:47]=[CH:46][CH:45]=[CH:44][CH:43]=3)[O:17][Si:16]([C:24]3[CH:29]=[CH:28][CH:27]=[CH:26][CH:25]=3)([C:18]3[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=3)[O:15][Si:14]([C:36]3[CH:41]=[CH:40][CH:39]=[CH:38][CH:37]=3)([C:30]3[CH:35]=[CH:34][CH:33]=[CH:32][CH:31]=3)[O:13]2)[CH:11]=[CH:10][CH:9]=[CH:8][CH:7]=1.C(N)CCCCC.Cl>O>[C:24]1([Si:16]([C:18]2[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=2)([OH:1])[O:17][Si:12]([C:42]2[CH:43]=[CH:44][CH:45]=[CH:46][CH:47]=2)([C:6]2[CH:11]=[CH:10][CH:9]=[CH:8][CH:7]=2)[O:13][Si:14]([C:36]2[CH:41]=[CH:40][CH:39]=[CH:38][CH:37]=2)([C:30]2[CH:31]=[CH:32][CH:33]=[CH:34][CH:35]=2)[OH:15])[CH:25]=[CH:26][CH:27]=[CH:28][CH:29]=1

Participants

6

Reactant 4

HCID 313Hydrochloric AcidHCID 8028TetrahydrofuranHCID 8102HexylamineHCID 68187Hexaphenylcyclotrisiloxane

Product 1

HCID 11982347HCID 11982347, compoundYield 93%

Reagents, catalysts & solvents 1

HCID 962WaterSolvent2×

Procedure

400 parts tetrahydrofuran and 55 parts hexaphenylcyclotrisiloxane were added to an Erlenmeyer flask, and dissolution was brought about. 3 parts hexylamine and 40 parts water were then added, and stirring was carried out for 30 minutes at room temperature. Conversion to the diol was confirmed by thin-layer chromatography, and the reaction solution was poured into 500 parts water and neutralized with dilute hydrochloric acid. The organic substance was precipitated with 600 parts of toluene, and this precipitate was repeatedly washed with water. Dehydration was then carried out with anhydrous sodium sulfate, and after filtration, the filtrate was condensed to 150 parts with a rotary evaporator. Hexane was then added to obtain crystals of hexaphenyltrisiloxane-1,5-diol in a yield of 93%.

Workup

  1. customThe organic substance was precipitated with 600 parts of toluene
  2. washthis precipitate was repeatedly washed with water
  3. filtrationafter filtration
  4. customcondensed to 150 parts
  5. customwith a rotary evaporator
  6. additionHexane was then added

Sources & evidence

ORD record
ord-9b2c8014921f4eeb95c71284aac44ca3
Source dataset
uspto-grants-1999_01
Patent number
US05861468

Reaction notes

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