4-Methylmorpholine → Cyclophosphamide

HRID 518591

反応式

HRID 518591 の反応式
[NH2:1][CH2:2][CH2:3][CH2:4][OH:5].CN1CCOCC1.[O:13]=[P:14](Cl)(Cl)Cl.Cl.[Cl:19][CH2:20][CH2:21][NH:22][CH2:23][CH2:24][Cl:25]>>[CH2:3]1[CH2:4][O:5][P:14]([N:22]([CH2:23][CH2:24][Cl:25])[CH2:21][CH2:20][Cl:19])(=[O:13])[NH:1][CH2:2]1

参加物

5

反応物 4

HCID 79724-MethylmorpholineHCID 90863-Amino-1-propanolHCID 24813Phosphorus oxychloride2 回HCID 522769Bis(2-chloroethyl)amine hydrochloride

生成物 1

HCID 2907Cyclophosphamide

実験手順

3-aminopropanol (2.1 g, 0.028 mol) and N-methylmorpholine (12.9 eq) are placed into a three-necked flask and stirred at room temperature. After cooling the mixture in the flask, POCl3 (4.3 g, 0.028 mol) is slowly dropped into the mixture. After adding POCl3, the mixture in the flask is stirred at room temperature for 15 hours. After that, bis(2-chloroethyl)amine hydrochloride] (5 g, 0.028 mol) is added into the mixture in the flask. The mixture in the flask is heated to about 40° C. and stirred for 6 hours. (The conversion yield determined with HPLC is about 10.0%.)

後処理

  1. additionis slowly dropped into the mixture
  2. stirringthe mixture in the flask is stirred at room temperature for 15 hours
  3. temperatureThe mixture in the flask is heated to about 40° C.
  4. stirringstirred for 6 hours
  5. custom(The conversion yield

出典と根拠

ORDレコード
ord-476edc016270404d86d4aa37bb45a02b
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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