HuagongsheHuagongshe Chemistry Print Report · For research reference only
1-Chloro-2,4-Dinitrobenzene → 4-Chloro-M-phenylenediamine
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | 1-Chloro-2,4-Dinitrobenzene | HCID 6 | — |
| Reactant | Water | HCID 962 | — |
| Reactant | Stannous chloride dihydrate | HCID 61436 | — |
| Reactant | Sodium Bicarbonate | HCID 516892 | — |
| Solvent | Ethanol | HCID 702 | — |
| Product | 4-Chloro-M-phenylenediamine | HCID 21209 | 110.8% |
Reaction Steps
A mixture of 1-chloro-2,4-dinitro-benzene (100 mg, 0.5 mmol) and SnCl2.2H2O (1.12 g, 5 mmol) in ethanol (2.5 mL) was stirred at room temperature overnight. Water was added and then the mixture was basified to pH 7-8 with saturated NaHCO3 solution. The solution was extracted with ethyl acetate. The combined organic layers were washed with brine, dried over Na2SO4, filtered and concentrated to yield 4-chloro-benzene-1,3-diamine (D-1) (79 mg, quant.). HPLC ret. time 0.38 min, 10-99% CH3CN, 5 min run; ESI-MS 143.1 m/z (MH+)
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08629162B2 |
| Source dataset | uspto-grants-2014_01 |
| ORD ID | ord-7810ffa4770444dd82486db763067234 |
| Source note | uspto-grants-2014_01 |