4-Chloro-6-hydrazinylpyrimidine → 4-Hydrazino-6-[4-(2-methoxyethyl)piperazin-1-yl]pyrimidine

HRID 242252

Reaction equation

Cl[C:2]1[CH:7]=[C:6]([NH:8][NH2:9])[N:5]=[CH:4][N:3]=1.[CH3:10][O:11][CH2:12][CH2:13][N:14]1[CH2:19][CH2:18][NH:17][CH2:16][CH2:15]1>O>[NH:8]([C:6]1[CH:7]=[C:2]([N:17]2[CH2:18][CH2:19][N:14]([CH2:13][CH2:12][O:11][CH3:10])[CH2:15][CH2:16]2)[N:3]=[CH:4][N:5]=1)[NH2:9]

Participants

Conditions

Temperature: 100 °C

Procedure

A mixture of 1.0 g (6.9 mmol) of the compound from Example 7A and 1.1 g (7.6 mmol) 1-(2-methoxyethyl)piperazine in 10 ml water is stirred at 100° C. for 2 h. A further 0.9 g (6.2 mmol) 1-(2-methoxyethyl)piperazine is added and the reaction mixture is stirred further at 100° C. for 16 h. After concentration in vacuo, the residue is stirred in acetonitrile. The solid which has precipitated out is filtered off, washed first with ethanol and then with diethyl ether and dried in vacuo.

Workup

stirringthe reaction mixture is stirred further at 100° C. for 16 h
concentrationAfter concentration in vacuo
stirringthe residue is stirred in acetonitrile
customThe solid which has precipitated out
filtrationis filtered off
washwashed first with ethanol
dry with materialwith diethyl ether and dried in vacuo

Sources & evidence

ORD record: ord-e264a4d9c3c84af5924e926533b54e99
Source dataset: uspto-grants-2014_02
DOI: 10.6084/m9.figshare.5104873.v1
Patent number: US08653111B2

Linked notes

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