1,4-Dimethylpiperazine → Cyclophosphamide

HRID 518592

反応式

HRID 518592 の反応式
Cl.[Cl:2][CH2:3][CH2:4][NH:5][CH2:6][CH2:7][Cl:8].CN1CCN(C)CC1.[O:17]=[P:18](Cl)(Cl)Cl.[NH2:22][CH2:23][CH2:24][CH2:25][OH:26]>>[CH2:24]1[CH2:25][O:26][P:18]([N:5]([CH2:6][CH2:7][Cl:8])[CH2:4][CH2:3][Cl:2])(=[O:17])[NH:22][CH2:23]1

参加物

5

反応物 4

HCID 78181,4-DimethylpiperazineHCID 90863-Amino-1-propanol2 回HCID 24813Phosphorus oxychlorideHCID 522769Bis(2-chloroethyl)amine hydrochloride

生成物 1

HCID 2907Cyclophosphamide

実験手順

Bis(2-chloroethyl)amine hydrochloride (5 g, 0.028 mol) is put into a 100 mL two-necked flask, and N,N′-Dimethylpiperazine (7.1 eq) is added into the flask. After cooling the flask and the reactants therein to about 4° C., POCl3 (4.49 g, 1.04 eq) is slowly dropped into the flask, and the mixture in the flask is stirred at room temperature for 5 hours. After that, the mixture in the flask is cooled to about 4° C., and 3-aminopropanol (2.1 g, 1.0 eq) is slowly dropped into the flask for 3 hours. After adding 3-aminopropanol into the flask, the mixture in the flask is stirred at room temperature for 15 hours. (The conversion yield determined with HPLC is about 11.84%.)

後処理

  1. temperatureAfter cooling the flask
  2. temperatureAfter that, the mixture in the flask is cooled to about 4° C.
  3. stirringthe mixture in the flask is stirred at room temperature for 15 hours
  4. custom(The conversion yield

出典と根拠

ORDレコード
ord-ae7cebbd395247038478627885df4fe9
出典データセット
uspto-grants-2015_08
特許番号
US09115160B2

関連ノート

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