HuagongsheHuagongshe Chemistry Print Report · For research reference only
Acetaldehyde → HCID 66755649, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Acetaldehyde | HCID 177 | — |
| Reactant | Triacetoxyborohydride | HCID 2724942 | — |
| Reactant | HCID 66754901 | HCID 66754901 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 66755649 | HCID 66755649 | — |
Reaction Steps
A solution of 99.0 mg (0.16 mmol) of 5-chloro-1-(4-methoxybenzenesulfonyl)-3-[2-oxo-1-phenyl-2-((S)-3-piperazin-1-yl-pyrrolidin-1-yl)ethyl]-1,3-dihydrobenzimidazol-2-one (example 149) in 4 ml of THF was mixed with 7.15 mg (0.16 mmol) of acetaldehyde and 160 mg of MP-triacetoxyborohydride resin (Argonaut, 2.55 mmol/g, 0.41 mmol) and shaken at room temperature overnight. The solid phase reagent was filtered off and washed with dichloromethane. The filtrate was concentrated under reduced pressure. The residue was purified by preparative RP-HPLC (mobile phase: gradient from 10% to 80% acetonitrile in water, 0.1% trifluoroacetic acid as modulator). Yield: 38.6 mg (38%) of colorless solid
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08119676B2 |
| Source dataset | uspto-grants-2012_02 |
| ORD ID | ord-6ad0df6235b64b399aab62795d9a1d30 |
| Source note | uspto-grants-2012_02 |