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Triethylamine → Cyclophosphamide

HRID 659310
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HRID 659310 반응식
[Cl:1][CH2:2][CH2:3][N:4]([CH2:9][CH2:10][Cl:11])[P:5](Cl)(Cl)=[O:6].CN[C:14]([C:18]1[CH:23]=CC=CC=1)([OH:17])CC.C([N:26](CC)CC)C>C(OCC)(=O)C>[CH2:18]1[CH2:14][O:17][P:5]([N:4]([CH2:9][CH2:10][Cl:11])[CH2:3][CH2:2][Cl:1])(=[O:6])[NH:26][CH2:23]1
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참가 물질

5

반응물 3

HCID 8471TriethylamineHCID 96271Phosphoramidic dichloride, bis(2-chloroethyl)-HCID 19933884Methylamino-1-phenyl-1-propanol

생성물 1

HCID 2907Cyclophosphamide

시약·촉매·용매 1

HCID 8857Ethyl Acetate용매2회

실험 절차

A solution of bis(2-chloroethyl)phosphoramidic dichloride (10 mmol) in ethyl acetate (100 mL) is added dropwise to a solution of commercial 3 methylamino-1-phenyl-1-propanol (10 mmol) and triethylamine (20 mmol) in ethyl acetate (100 mL) at rt. After stirring at rt for 3 days, the salts are filtered off and the combined filtrates are concentrated under vacuum. The crude product is purified by column chromatography on silica.

후처리

  1. filtrationthe salts are filtered off
  2. concentrationthe combined filtrates are concentrated under vacuum
  3. customThe crude product is purified by column chromatography on silica

출처 및 근거

ORD 기록
ord-ba24910390c54d239897abdfb963ae7b
출처 데이터셋
uspto-grants-2011_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08080536B2

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