Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Acetic Acid | HCID 176 | — |
| Reactant | Acetaldehyde | HCID 177 | — |
| Reactant | Sodiumacetoxyborohydride | HCID 23670382 | — |
| Reactant | HCID 68777299 | HCID 68777299 | — |
| Solvent | Methanol | HCID 887 | — |
| Product | HCID 68764844 | HCID 68764844 | 98% |
Reaction Steps
To a suspension of 3-{7-amino-2-[(2,4-dichlorophenyl)amino]-5-fluoro-1H-benzimidazol-1-yl}propan-1-ol (369 mg, 1.00 mmol) and acetic acid (0.5 mL) in methanol (10 mL) was added acetoaldehyde (374 μL, 6.00 mmol) at room temperature. After 30 min, sodium acetoxyborohydride (1.27 g, 6.00 mmol) was added. After 4 h, the mixture was cooled down to 0° C. Then acetic acid (0.5 mL) and acetoaldehyde (374 μL, 6.00 mmol) was added. After 30 min, sodium acetoxyborohydride (1.27 g, 6.00 mmol) was added. After 1 h, the reaction mixture was quenched with water, concentrated in vacuo, diluted with ethyl acetate, washed with aqueous sodium hydroxide (1 M) and brine, dried over sodium sulfate, filtered and concentrated in vacuo to give the title compound as a solid (408 mg, 0.983 mmol, 98%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US08901141B2 |
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| Source dataset | uspto-grants-2014_12 |
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| ORD ID | ord-ed9f7a0aacc340048f7bee19fb4e4c40 |
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| Source note | uspto-grants-2014_12 |
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