Potassium Carbonate → HCID 17968201, compound
Reaction equation
Br[CH2:2][C:3]1[N:13]([CH2:14][C:15]([CH3:18])([CH3:17])[CH3:16])[C:6]2[N:7]=[C:8]([C:11]#[N:12])[N:9]=[CH:10][C:5]=2[CH:4]=1.Cl.Cl.[CH3:21][N:22]([CH3:38])[CH2:23][CH2:24][O:25][C:26]1[CH:31]=[CH:30][C:29]([CH:32]2[CH2:37][CH2:36][NH:35][CH2:34][CH2:33]2)=[CH:28][CH:27]=1.C(=O)([O-])[O-].[K+].[K+]>CC(C)=O>[CH3:21][N:22]([CH3:38])[CH2:23][CH2:24][O:25][C:26]1[CH:31]=[CH:30][C:29]([CH:32]2[CH2:37][CH2:36][N:35]([CH2:2][C:3]3[N:13]([CH2:14][C:15]([CH3:18])([CH3:17])[CH3:16])[C:6]4[N:7]=[C:8]([C:11]#[N:12])[N:9]=[CH:10][C:5]=4[CH:4]=3)[CH2:34][CH2:33]2)=[CH:28][CH:27]=1Participants
5
Procedure
0.22 g of 6-bromomethyl-7-(2,2-dimethyl-propyl)-7H-pyrrolo[2,3-d]pyrimidine-2-carbonitrile, 0.23 g of dimethyl-[2-(4-piperidin-4-yl-phenoxy)-ethyl]-amine bishydrochloride and 0.5 g of potassium carbonate were stirred in 2 ml acetone at 25° C. for 2 hours. The mixture was extracted with ethyl acetate/water, dried over sodium sulfate and evaporated to driness. After chromatography on silicagel using CH2Cl2/MeOH=90:10 6-{4-[4-(2-dimethylamino-ethoxy)-phenyl]-piperidin-1-ylmethyl}-7-(2,2-dimethyl-propyl)-7H-pyrrolo[2,3-d]pyrimidine-2-carbonitrile was obtained as yellow solid.
Workup
- extractionThe mixture was extracted with ethyl acetate/water
- dry with materialdried over sodium sulfate
- customevaporated to driness
- customwas obtained as yellow solid
Sources & evidence
- ORD record
- ord-f476352b6d4248e5bdac2a069485da77
- Source dataset
- uspto-grants-2008_11
- Patent number
- US07452886B2
Reaction notes
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