Hydrochloric Acid → HCID 22329462, compound

HRID 586417Notes

Reaction equation

HRID 586417 reaction equation
[CH2:1]([N:8]1[CH2:13][CH2:12][N:11]([C:14]2[N:19]=[C:18]([NH:20][C:21]3[CH:26]=[CH:25][C:24]([Cl:27])=[C:23]([Cl:28])[CH:22]=3)[CH:17]=[C:16]([N:29]3[CH2:38][CH2:37][C:32]4(OCC[O:33]4)[CH2:31][CH2:30]3)[N:15]=2)[CH2:10][CH2:9]1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.Cl>O1CCOCC1>[CH2:1]([N:8]1[CH2:9][CH2:10][N:11]([C:14]2[N:15]=[C:16]([N:29]3[CH2:30][CH2:31][C:32](=[O:33])[CH2:37][CH2:38]3)[CH:17]=[C:18]([NH:20][C:21]3[CH:26]=[CH:25][C:24]([Cl:27])=[C:23]([Cl:28])[CH:22]=3)[N:19]=2)[CH2:12][CH2:13]1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1

Participants

4

Reactant 2

HCID 313Hydrochloric AcidHCID 22329434HCID 22329434, compound

Product 1

HCID 22329462HCID 22329462, compoundYield 11%

Reagents, catalysts & solvents 1

HCID 312751,4-DioxaneSolvent

Procedure

A mixture of 2-(4-benzyl-1-piperazinyl)-N-(3,4-dichlorophenyl)-6-(1,4-dioxa-8-azaspiro[4.5]dec-8-yl)-4-pyrimidinamine (100 mg, 0.18 mmol) and 4M HCl (10 mL) in dioxane (20 mL) was stirred at room temperature for 24 hours. The crude product was purified by preparative thin-layer chromatography [eluent: EtOAc/hexane (2:3) with 1% NH3 in methanol], giving the desired product (10 mg, 11%).

Workup

  1. customThe crude product was purified by preparative thin-layer chromatography [eluent: EtOAc/hexane (2:3) with 1% NH3 in methanol]

Sources & evidence

ORD record
ord-a05ecef65a86480e91269b0efb95a0c3
Source dataset
uspto-grants-2005_08
Patent number
US06936607B2

Reaction notes

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