Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | Sarcosine methyl ester | HCID 83545 | — |
| Reactant | Biotin | HCID 171548 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | HCID 131721605 | HCID 131721605 | — |
Reaction Steps
To a solution of biotin in anhydrous dimethylformamide is added 1.1 equivalents of N-methylglycine methyl ester and 3 equivalents of triethylamine followed by the addition of 1.05 equivalents of BOP (benzotriazol-1-yloxy-tris (dimethylamine)phosphonium hexafluorophosphate). The mixture is stirred at 0-25° C. for 2-24 h and then concentrated. The residue is diluted with ethyl acetate and the resulting solution is washed with 1 N aqueous hydrochloric acid and then with saturated aqueous sodium bicarbonate. The organic phase is dried over magnesium sulfate, filtered and then concentrated via reduced pressure rotary evaporation. The residue is chromatographed on silica gel, eluting with 5-15% methanol/ethyl acetate. Chromatographic fractions containing product are combined and concentrated to afford the final product (4).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US06217869B1 |
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| Source dataset | uspto-grants-2001_04 |
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| ORD ID | ord-b7b5d8f7633c434687b7ae9f00af2d45 |
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| Source note | uspto-grants-2001_04 |
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