Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Thiazolidine | HCID 10444 | — |
| Reactant | Diisopropylethylamine | HCID 81531 | — |
| Reactant | HCID 57945112 | HCID 57945112 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | HCID 57945087 | HCID 57945087 | 67% |
Reaction Steps
A solution of 35 mg (0.046 mmol) of (3R,3aS,6aR)-hexahydrofuro[2,3-b]furan-3-yl (1S,2R)-3-[(1,3-benzodioxol-5-ylsulfonyl)(isobutyl)amino]-2-hydroxy-1-[4-(3-iodopropoxy)benzyl]propylcarbamate, 11 μL (0.14 mmol) of thiazolidine, and 32 μL (0.18 mmol) of N,N-diisopropylethylamine in 0.5 mL of anhydrous DMF was heated to 80° C. with stirring. After 1.5 hours TLC indicated the reaction to be complete. The solution was cooled to RT and concentrated in vacuo. The residue was subjected to flash chromatography (SiO2, 95:5 CH2Cl2/MeOH) to afford 22 mg (67%) of the desired compound as a white foam. 1H NMR (CDCl3): 7.29 (d, 1H), 7.13 (s, 1H), 7.08 (d, 2H), 7.85 (d, 1H), 6.77 (d, 2H), 6.04 (s, 2H), 5.60 (d, 1H), 5.00 (q, 1H), 4.88 (d, 1H), 4.01 (s, 2H), 4.00-3.88 (m, 3H), 3.80 (m, 3H), 3.67 (m, 2H), 3.55 (br s, 1H), 3.19-3.01 (m, 4H), 3.00-2.65 (m, 7H), 2.52 (t, 2H), 1.93 (m, 2H), 1.79 (m, 1H), 1.70-1.42 (m, 2H), 0.89 (d, 3H), 0.83 (d, 3H). MS(ESI): 722(M+H).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US06878728B1 |
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| Source dataset | uspto-grants-2005_04 |
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| ORD ID | ord-399c2d67dd7f4449b69e0bb9eef0c762 |
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| Source note | uspto-grants-2005_04 |
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