Trichloroacetic Acid → 2-[2-(bis-(2-chloroethyl)-amino)-2-oxo-tetrahydro-2H-1,3,2-oxazaphosphorin-3-yl-thio]-ethanesulphonic acid ammonium salt

HRID 1651520

反応式

HRID 1651520 の反応式
[CH2:1]1[CH:7](O)[NH:6][P:4]([N:9]([CH2:13][CH2:14][Cl:15])[CH2:10][CH2:11][Cl:12])(=[O:5])[O:3][CH2:2]1.[NH4+].[SH:17][CH2:18][CH2:19][S:20]([O-:23])(=[O:22])=[O:21].ClC(Cl)(Cl)C(O)=O>CN(C)C=O>[NH4+:6].[Cl:12][CH2:11][CH2:10][N:9]([CH2:13][CH2:14][Cl:15])[P:4]1(=[O:5])[N:6]([S:17][CH2:18][CH2:19][S:20]([O-:23])(=[O:22])=[O:21])[CH2:7][CH2:1][CH2:2][O:3]1

参加物

5

反応物 3

HCID 6421Trichloroacetic AcidHCID 997354-HydroxycyclophosphamideHCID 23049872Ammonium 2-mercaptoethanesulphonate

生成物 1

HCID 886069922-[2-(bis-(2-chloroethyl)-amino)-2-oxo-tetrahydro-2H-1,3,2-oxazaphosphorin-3-yl-thio]-ethanesulphonic acid ammonium salt

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

2.8 g (10 mmol), of 4-hydroxycyclophosphamide and 1.6 g (10 mmol) of ammonium-2-mercaptoethanesulphonate were dissolved with a cataytic quantity of trichloroacetic acid in 10 ml of dimethylformamide and were stored in a refrigerator at -25° C. for 20 hours. After a further 5 hours at 0° C., the mixture was mixed with ehter until clouding commenced and was triturbated. The crystrallised material was filtered with suction after 1 day at 0° C., washed dried and recrystallised from n-propanol.

後処理

  1. waitAfter a further 5 hours at 0° C.
  2. additionthe mixture was mixed with ehter
  3. filtrationThe crystrallised material was filtered with suction after 1 day at 0° C.
  4. washwashed
  5. customdried
  6. customrecrystallised from n-propanol

出典と根拠

ORDレコード
ord-a47512727d894a65a6de4a9b588f000e
出典データセット
uspto-grants-1990_05
特許番号
US04929607

関連ノート

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