Hydrochloric Acid → HCID 67515777, compound

Temperature

90 °C

In a 15 mL microwave reaction vial, was added methyl 5-bromo-3-(bromomethyl)thiophene-2-carboxylate (700 mg, 2.23 mmol), THF (4 mL) and MeOH (1 mL). To above solution was added lithium hydroxide (53.4 mg, 2.23 mmol, 1.0 eq) in water (1 mL). The reaction was heated in microwave reactor for 30 min at 90° C. The reaction was cooled down to r.t., neutralized with 1N HCl, extracted with EtOAc, washed with brine and water. The organic phase was dried over MgSO4, filtered and concentrated. The desired product was obtained after purification by flash column chromatography. LC-MS (IE, m/z): 235.2 [M+1]+.

1. customIn a 15 mL microwave reaction vial
2. temperatureThe reaction was cooled down to r.t.
3. extractionextracted with EtOAc
4. washwashed with brine and water
5. dry with materialThe organic phase was dried over MgSO4
6. filtrationfiltered
7. concentrationconcentrated

ORD record

ord-38875e088f4a463fb23b5d615295eadc

Source dataset

uspto-grants-2015_06

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US09056859B2