Diethyl Ether → 2-[2-(bis-(2-chloroethyl)-amino)-2-oxo-tetrahydro-2H-1,3,2-oxazaphosphorin-4-yl-thio]-ethanesulphonic acid ammonium salt

HRID 1731965

反応式

HRID 1731965 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.CCOCC>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])[NH:6][CH:7]([S:17][CH2:18][CH2:19][S:20]([O-:23])(=[O:22])=[O:21])[CH2:1][CH2:2][O:3]1

参加物

6

反応物 4

HCID 3283Diethyl EtherHCID 6421Trichloroacetic AcidHCID 997354-HydroxycyclophosphamideHCID 23049872Ammonium 2-mercaptoethanesulphonate

生成物 1

HCID 1101861772-[2-(bis-(2-chloroethyl)-amino)-2-oxo-tetrahydro-2H-1,3,2-oxazaphosphorin-4-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 catalytic 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 ether until clouding commenced and was triturated. The crystallised 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. customwas triturated
  3. filtrationThe crystallised 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-fc093a1fd6cb4ff5a55007168b77f9f8
出典データセット
uspto-grants-1986_11
特許番号
US04623742

関連ノート

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