HuagongsheHuagongshe Chemistry Print Report · For research reference only
Trifluoroacetic acid → HCID 18442588, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Trifluoroacetic acid | HCID 6422 | — |
| Reactant | Dichloromethane methanol | HCID 21226129 | — |
| Reactant | Sodium hydroxide--water (1/1/1) | HCID 23719242 | — |
| Reactant | HCID 69353488 | HCID 69353488 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 18442588 | HCID 18442588 | 47.5% |
Reaction Steps
To a stirred solution of 9-(3,4-dimethoxy-benzyl)-2,3-dimethoxy-5,5-dioxo-5,6,7,9 tetrahydro-5λ6-thia-8-aza-benzocycloheptene-8-carboxylic acid tert-butyl ester (310 mg, 0.61 mmol) in dry CH2Cl2 (3 ml), was added trifluoroacetic acid (372 μL, 4.86 mmol). The resulting mixture was stirred at RT for 20 h under nitrogen. The reaction mixture was combined with water/NaOH 2N, extracted twice with CH2Cl2, and the combined organic phases were dried over anhydrous MgSO4, filtered and concentrated to give a crude oil. Flash chromatography (CH2Cl2/MeOH: 9/1) gave the title compound as a pale yellow oil (118 mg, 47%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07192950B2 |
| Source dataset | uspto-grants-2007_03 |
| ORD ID | ord-db114610e907493e8e4ba196fd867258 |
| Source note | uspto-grants-2007_03 |