Hydrochloric Acid → Hydrochloric Acid

HRID 2090481Notes

Reaction equation

HRID 2090481 reaction equation
[NH2:1][C:2]1[N:7]=[C:6]([N:8]2[CH:17]([CH3:18])[CH2:16][C:15]3[C:10](=[CH:11][C:12]([C:19]4[CH2:20][CH2:21][N:22](C(OC(C)(C)C)=O)[CH2:23][CH:24]=4)=[CH:13][CH:14]=3)[CH2:9]2)[CH:5]=[C:4]([N:32]2[CH2:37][CH2:36][N:35]([CH3:38])[CH2:34][CH2:33]2)[N:3]=1.[ClH:39].O1CCOCC1>C(OCC)(=O)C.C(OCC)C>[CH3:38][N:35]1[CH2:36][CH2:37][N:32]([C:4]2[CH:5]=[C:6]([N:8]3[CH:17]([CH3:18])[CH2:16][C:15]4[C:10](=[CH:11][C:12]([C:19]5[CH2:20][CH2:21][NH:22][CH2:23][CH:24]=5)=[CH:13][CH:14]=4)[CH2:9]3)[N:7]=[C:2]([NH2:1])[N:3]=2)[CH2:33][CH2:34]1.[ClH:39]

Participants

7

Reactant 3

HCID 313Hydrochloric AcidHCID 312751,4-DioxaneHCID 59402271HCID 59402271, compound

Product 2

HCID 313Hydrochloric AcidHCID 59402262HCID 59402262, compound

Reagents, catalysts & solvents 2

HCID 3283Diethyl EtherSolventHCID 8857Ethyl AcetateSolvent

Procedure

tert-Butyl 4-{2-[2-amino-6-(4-methylpiperazin-1-yl)pyrimidin-4-yl]-3-methyl-1,2,3,4-tetrahydroisoquinolin-7-yl}-3,6-dihydropyridine-1(2H)-carboxylate (0.20 g, 0.38 mmol) in ethyl acetate (1.0 mL) was treated with 4.0 M of hydrogen chloride in 1,4-dioxane (1.0 mL, 4.0 mmol) at r.t. for 2 h. The mixture was diluted with ethyl ether, and centrifugalized. The solvents were decanted. The residue was dried in-vacuo to afford the desired product as HCl salt which was directly used in next step reaction without further purification. LCMS (M+H)+: m/z=420.2.

Workup

  1. customThe solvents were decanted
  2. customThe residue was dried in-vacuo

Sources & evidence

ORD record
ord-41839abb654348628b4828714f76ec00
Source dataset
uspto-grants-2013_05
Patent number
US08436008B2

Reaction notes

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