Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Diethyl Ether → 2-[2-(bis-(2-chloroethyl)-amino)-2-oxo-tetrahydro-2H-1,3,2-oxazaphosphorin-4-yl-thio]-ethanesulphonic acid ammonium salt
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Diethyl Ether | HCID 3283 | — |
| 반응물 | Trichloroacetic Acid | HCID 6421 | — |
| 반응물 | 4-Hydroxycyclophosphamide | HCID 99735 | — |
| 반응물 | Ammonium 2-mercaptoethanesulphonate | HCID 23049872 | — |
| 용매 | Dimethylformamide | HCID 6228 | — |
| 생성물 | 2-[2-(bis-(2-chloroethyl)-amino)-2-oxo-tetrahydro-2H-1,3,2-oxazaphosphorin-4-yl-thio]-ethanesulphonic acid ammonium salt | HCID 110186177 | — |
반응 단계
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.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US04623742 |
| 출처 데이터셋 | uspto-grants-1986_11 |
| ORD ID | ord-fc093a1fd6cb4ff5a55007168b77f9f8 |
| 출처 메모 | uspto-grants-1986_11 |