Chlorotrimethylsilane → HCID 21453166, compound

HRID 1282820Notes

Reaction equation

HRID 1282820 reaction equation
[NH:1]1[CH2:6][CH2:5][CH2:4][NH:3][C:2]1=[O:7].C[Si](C)(C)Cl.C(N(CC)CC)C.[O:20]1CCOC[CH2:21]1>>[CH:21]([N:1]1[CH2:6][CH2:5][CH2:4][NH:3][C:2]1=[O:7])=[O:20]

Participants

5

Reactant 4

HCID 6397ChlorotrimethylsilaneHCID 8471TriethylamineHCID 312751,4-DioxaneHCID 746152(1H)-Pyrimidinone, tetrahydro-

Product 1

HCID 21453166HCID 21453166, compound

Procedure

The mixture of 10 parts by weight of 1,3-diaza-cyclohexane-2-one, 49 parts by weight of trimethylchlorosilane, 25 parts by weight of triethylamine and 150 parts by volume of dioxane were boiled for 3 days with stirring and exclusion of moisture, then filtered, evaporated to 50 parts by volume in vacuo and stirred overnight with 11.5 parts by volume of formic acid-acetic acid anhydride. The mixture was evaporated to dryness in vacuo, and the residue was recrystallized from ethanol/ether.

Workup

  1. filtrationexclusion of moisture, then filtered
  2. customevaporated to 50 parts by volume in vacuo
  3. stirringstirred overnight with 11.5 parts by volume of formic acid-acetic acid anhydride
  4. customThe mixture was evaporated to dryness in vacuo
  5. customthe residue was recrystallized from ethanol/ether

Sources & evidence

ORD record
ord-6a3670ac65784f309e5d472d55f3a327
Source dataset
uspto-grants-1976_08
Patent number
US03972869

Reaction notes

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