HuagongsheHuagongshe Chemistry Print Report · For research reference only
Diethyl Ether → ASTA-Z-7654(free acid)
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Diethyl Ether | HCID 3283 | — |
| Reactant | Trichloroacetic Acid | HCID 6421 | — |
| Reactant | 2-Sulfanylethane-1-sulfonic acid--cyclohexanamine (1/1) | HCID 23049873 | — |
| Reactant | 2-(bis-(2-chloroethyl)-amino)-4-methoxy-tetrahydro-2H-1,3,2-oxazaphosphorin-2-oxide | HCID 23049879 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | ASTA-Z-7654(free acid) | HCID 6917796 | — |
Reaction Steps
2.9 g (10 mmol) of 2-(bis-(2-chloroethyl)-amino)-4-methoxy-tetrahydro-2H-1,3,2-oxazaphosphorin-2-oxide and 2.4 g (10 mmol) of cyclohexylammonium-2-mercaptoethanesulphonate were dissolved with some trichloroacetic acid in 10 ml of dimethylformamide and were stored at -25° C. for 20 hours. After leaving the mixture to stand for another three hours at 0° C., it was mixed with ether until clouding commenced, triturated, the crystallised material was filtered with suction after standing for 20 hours at 0° C., and was washed and dried.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US04623742 |
| Source dataset | uspto-grants-1986_11 |
| ORD ID | ord-3ca5ca98e1404661871237c0ae6e7762 |
| Source note | uspto-grants-1986_11 |