HuagongsheHuagongshe Chemistry Print Report · For research reference only
Ammonia → HCID 67304797, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Ammonia | HCID 222 | — |
| Reactant | HCID 86630948 | HCID 86630948 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 67304797 | HCID 67304797 | 118% |
Reaction Steps
To a solution of the above prepared 4-(2-methoxy-ethyl)-5-methyl-thiophene-2-sulfonyl chloride (4.59 g, 18 mmol) in DCM (18 mL) were added 25% aqueous NH3 (9 mL, ˜120 mmol) and the biphasic reaction mixture was vigorously stirred at rt for 3 h. After the addition of DCM (120 mL) the reaction mixture was washed with H2O (2×120 mL) and the aqueous layers were extracted with DCM (50 mL). The combined organic layers were dried (Na2SO4) and evaporated affording 5.0 g crude product as a yellow viscous oil which was purified by chromatography over silica with hexane-ethyl acetate 2:1 providing 3.62 g (85% GC 96.3%) yellow viscous oil. ESI-MS (m/z) 253 (M+NH4+, 100).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07973051B2 |
| Source dataset | uspto-grants-2011_07 |
| ORD ID | ord-9b818de1bb7142e8ac3988db6aed6e5c |
| Source note | uspto-grants-2011_07 |