HuagongsheHuagongshe Chemistry Print Report · For research reference only
Water → N'-Methyl-2-(2-methyl-2-(phenylcarbonothioyl)hydrazinyl)-2-oxo-N'-(phenylcarbonothioyl)ethanesulfonohydrazide
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Water | HCID 962 | — |
| Reactant | (Chlorosulphonyl)acetyl chloride | HCID 77642 | — |
| Reactant | N-methylbenzothiohydrazide | HCID 12206211 | — |
| Solvent | Pyridine | HCID 1049 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | N'-Methyl-2-(2-methyl-2-(phenylcarbonothioyl)hydrazinyl)-2-oxo-N'-(phenylcarbonothioyl)ethanesulfonohydrazide | HCID 59267374 | 36.6% |
Reaction Steps
To a 0° C. solution of N-methylbenzothiohydrazide (10 mmol) in DCM (20 mL) and pyridine (1 mL) was added 2-(chlorosulfonyl)acetyl chloride (5 mmol) dropwise. The mixture was kept at rt for 2 h before it was poured into water (20 ml). The organic layer was separated, dried and evaporated and the resulting residue was purified by column chromatography to give compound 68 as yellowish solids (0.8 g). 1H-NMR (CDCl3) δ 10.5 (m, 1H), 7.4 (m, 10H), 4.4 (m, 1H), 3.4-3.8 (m, 8H) ppm; ESMS calcd for C18H20N4O3S3:436.1; found: 437.2 (M+H+).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08609720B2 |
| Source dataset | uspto-grants-2013_12 |
| ORD ID | ord-c7727f6a340942459d6d02d38eb31441 |
| Source note | uspto-grants-2013_12 |