Chlorotrimethylsilane → HCID 21453166, compound

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

Reactant 4

HCID 6397Chlorotrimethylsilane

HCID 8471Triethylamine

HCID 312751,4-Dioxane

HCID 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

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

Sources & evidence

ORD record: ord-6a3670ac65784f309e5d472d55f3a327
Source dataset: uspto-grants-1976_08
DOI: 10.6084/m9.figshare.5104873.v1
Patent number: US03972869

Reaction notes

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