Potassium Carbonate → HCID 67258462, compound

HRID 1476633Notes

Reaction equation

[O:1]=[C:2]1[NH:7][C:6]2[CH:8]=[C:9]([C:11]3[CH:16]=[CH:15][CH:14]=[CH:13][CH:12]=3)[S:10][C:5]=2[C:4](=[O:17])[N:3]1[CH:18]1[CH2:23][CH2:22][N:21]([C:24]([O:26][C:27]([CH3:30])([CH3:29])[CH3:28])=[O:25])[CH2:20][CH2:19]1.Cl.Cl[CH2:33][C:34]1[N:35]([CH3:39])[CH:36]=[CH:37][N:38]=1.C(=O)([O-])[O-].[K+].[K+]>CN(C=O)C>[CH3:39][N:35]1[CH:36]=[CH:37][N:38]=[C:34]1[CH2:33][N:7]1[C:6]2[CH:8]=[C:9]([C:11]3[CH:16]=[CH:15][CH:14]=[CH:13][CH:12]=3)[S:10][C:5]=2[C:4](=[O:17])[N:3]([CH:18]2[CH2:23][CH2:22][N:21]([C:24]([O:26][C:27]([CH3:30])([CH3:29])[CH3:28])=[O:25])[CH2:20][CH2:19]2)[C:2]1=[O:1]

Participants

Conditions

Temperature: 50 °C

Procedure

To a solution of tert-butyl 4-(2,4-dioxo-6-phenyl-1,4-dihydrothieno[3,2-d]pyrimidin-3(2H)-yl)piperidine-1-carboxylate (1.16 g, compound B50) and 2-(chloromethyl)-1-methyl-1H-imidazole hydrochloride (500 mg, compound D31) in dry DMF (15 ml) is added potassium carbonate (753 mg). The mixture is stirred for 3 h at 50° C. and subsequently poured into ice-cold water. After stirring for 5 min the resulting precipitate is filtered off and dried in vacuo. The residue is taken up in EtOAc, filtered off and dried in vacuo to afford the title compound as a solid

Workup

additionsubsequently poured into ice-cold water
stirringAfter stirring for 5 min the resulting precipitate
filtrationis filtered off
customdried in vacuo
filtrationfiltered off
customdried in vacuo

Sources & evidence

ORD record: ord-48292be2a0fb41b0ac72b729cc016b5e
Source dataset: uspto-grants-2015_04
DOI: 10.6084/m9.figshare.5104873.v1
Patent number: US09018175B2

Reaction notes

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