HuagongsheHuagongshe Chemistry Print Report · For research reference only
Methanol → HCID 22609710, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Methanol | HCID 887 | — |
| Reactant | Potassium bisulfate | HCID 516920 | — |
| Reactant | HCID 22609837 | HCID 22609837 | — |
| Reactant | Potassium hydroxy sulfite | HCID 23707502 | — |
| Solvent | Water | HCID 962 | — |
| Product | HCID 22609710 | HCID 22609710 | 52% |
Reaction Steps
A solution of N-(2-methylthioethyl)trifluoroacetamide (19.0 g, 109.7 mmol) in methanol (200 ml) was cooled to 0° C. using an ice bath. A suspension of Oxone™ (2KHSO5.KHSO4.K2SO4) (74.19 g, 120.67 mmol) in water (100 ml) was added portionwise over 10 minutes, and the reaction was stirred at room temperature for 24 hours. The methanol was removed in vacuo, water (600 ml) was added and the mixture was extracted with dichloromethane (3×300 ml). The combined extracts were dried (MgSO4), and concentrated in vacuo to give the title compound as a white solid (12.42 g, 56.7 mmol, 52%); δH CDCl3 7.33 (1H,br s), 3.93 (2H,q), 3.31 (2H,t), 3.02 (3H,s).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06391874B1 |
| Source dataset | uspto-grants-2002_05 |
| ORD ID | ord-f699edbee2854b4d9098a39b3507290f |
| Source note | uspto-grants-2002_05 |