HuagongsheHuagongshe Chemistry Print Report · For research reference only
Sodium methanethiolate → 7-Hydroxy-6-methoxy-2-methylsulfanyl-3-(3,4,5-trimethoxybenzoyl)benzofuran
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Sodium methanethiolate | HCID 4378561 | — |
| Reactant | 2-Bromo-7-acetoxy-3-(3,4,5-trimethoxybenzoyl)-6-methoxybenzofuran | HCID 24786560 | — |
| Solvent | Methanol | HCID 887 | — |
| Product | 7-Hydroxy-6-methoxy-2-methylsulfanyl-3-(3,4,5-trimethoxybenzoyl)benzofuran | HCID 24880049 | — |
Reaction Steps
To a suspension of 2-Bromo-7-acetoxy-3-(3,4,5-trimethoxybenzoyl)-6-methoxybenzofuran (22 mg, 0.046 mmol) in methanol (1 ml) in a screw cap vial was added sodium thiomethoxide (16 mg, 0.23 mmol) and the resulting orange solution was shaken for 20 minutes during which time the reaction became homogeneous. The crude reaction mixture was concentrated onto silica and chromatographed (silica gel, eluent=2:1 hexanes:ethyl acetate) to give the product as a resin (10 mg, 54%) that could be crystallised by standing in hexanes in the freezer overnight; 1H NMR (CDCl3) δ 7.08 (s, 2H), 6.92 (d, J=8.3 Hz, 1H), 6.82 (d, J=8.3 Hz, 1H), 5.73 (br s, 1H), 3.93 (s, 3H), 3.92 (s, 3H), 3.84 (s, 6H), 2.66 (s, 3H).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08198466B2 |
| Source dataset | uspto-grants-2012_06 |
| ORD ID | ord-299b1ac2b5544b22bfe91c4ccd52b9c9 |
| Source note | uspto-grants-2012_06 |