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

HRID 242252

反応式

HRID 242252 の反応式
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]

参加物

4

反応物 2

HCID 2472224-Chloro-6-hydrazinylpyrimidineHCID 27346381-(2-Methoxyethyl)piperazine2 回

生成物 1

HCID 596036074-Hydrazino-6-[4-(2-methoxyethyl)piperazin-1-yl]pyrimidine

試薬・触媒・溶媒 1

HCID 962Water溶媒

反応条件

温度
100 °C

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-e264a4d9c3c84af5924e926533b54e99
出典データセット
uspto-grants-2014_02
特許番号
US08653111B2

関連ノート

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