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

HRID 1942005

Reaction equation

HRID 1942005 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

4

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

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

Sources & evidence

ORD record
ord-bb195120b6e14d75b6ea961269b809ce
Source dataset
uspto-grants-2013_03
Patent number
US08389520B2

Linked notes

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