Trichlorosilane → HCID 87410090, compound

HRID 1949620Notes

Reaction equation

HRID 1949620 reaction equation
[SiH:1]([Cl:4])([Cl:3])[Cl:2].[CH2:5]([C:8]1[CH:13]=[CH:12][C:11]([N:14]([C:41]2[CH:46]=[CH:45][CH:44]=[CH:43][CH:42]=2)[C:15]2[S:19][C:18]([C:20]3[S:21][C:22]([N:25]([C:32]4[CH:37]=[CH:36][C:35]([CH2:38][CH:39]=[CH2:40])=[CH:34][CH:33]=4)[C:26]4[CH:31]=[CH:30][CH:29]=[CH:28][CH:27]=4)=[CH:23][CH:24]=3)=[CH:17][CH:16]=2)=[CH:10][CH:9]=1)[CH:6]=[CH2:7]>C1(C)C=CC=CC=1.C1([Pt-](Cl)C2C=CC=C2)C=CC=C1>[Cl:2][Si:1]([CH2:40][CH2:39][CH2:38][C:35]1[CH:34]=[CH:33][C:32]([N:25]([C:26]2[CH:31]=[CH:30][CH:29]=[CH:28][CH:27]=2)[C:22]2[S:21][C:20]([C:18]3[S:19][C:15]([N:14]([C:11]4[CH:10]=[CH:9][C:8]([CH2:5][CH2:6][CH2:7][Si:1]([Cl:4])([Cl:3])[Cl:2])=[CH:13][CH:12]=4)[C:41]4[CH:42]=[CH:43][CH:44]=[CH:45][CH:46]=4)=[CH:16][CH:17]=3)=[CH:24][CH:23]=2)=[CH:37][CH:36]=1)([Cl:4])[Cl:3]

Participants

5

Reactant 2

HCID 24811TrichlorosilaneHCID 68659281HCID 68659281, compound

Product 1

HCID 87410090HCID 87410090, compound

Reagents, catalysts & solvents 2

HCID 178479807HCID 178479807, compoundCatalystHCID 1140TolueneSolvent

Conditions

Temperature
60 °C

Procedure

Excess HSiCl3 (0.09 mL, 8.609×10−4 mol) and a few grains of dicyclopentadienylplatinum(II) chloride (Cp2PtCl2) catalyst were added in a glove box to a solution of Compound 4 (0.050 g, 8.609×10−5 mol) in about 10 mL anhydrous toluene. The solution was transferred to a Schlenk line where it was heated to 60° C. with stirring and left under static N2 to prevent evaporation of the HSiCl3. The reaction progress was monitored by 1H NMR, and cooled to room temperature after 42 h. Toluene and excess HSiCl3 were next removed in vacuo. Upon trituration of the crude product with 15 mL of a dry 1:1 toluene:pentane solution, a solid formed and was removed via cannula filtration.

Workup

  1. customThe solution was transferred to a Schlenk
  2. waitleft under static N2
  3. customevaporation of the HSiCl3
  4. temperaturecooled to room temperature after 42 h
  5. customToluene and excess HSiCl3 were next removed in vacuo
  6. dry with materialUpon trituration of the crude product with 15 mL of a dry 1:1 toluene
  7. custompentane solution, a solid formed
  8. customwas removed via cannula filtration

Sources & evidence

ORD record
ord-4975d87f281e428a984769fd4c37af49
Source dataset
uspto-grants-2013_03
Patent number
US08399761B2

Reaction notes

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