HuagongsheHuagongshe Chemistry Print Report · For research reference only
Formaldehyde → HCID 18771958, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Formaldehyde | HCID 712 | — |
| Reactant | Sodium triacetoxyborohydride | HCID 5049666 | — |
| Reactant | HCID 18771846 | HCID 18771846 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 18771958 | HCID 18771958 | — |
Reaction Steps
A mixture of N-[2-(4-pyridinyl)-4-thiazolyl]-N′-2-[6-(4-piperidinylethoxy)pyridinyl]urea (0.17 g, 0.40 mmol, Example 167), paraformaldehyde (0.17 g), and NaBH(OAc)3 (0.21 g, 1.0 mmol) in 40 mL of CH2Cl2 was stirred at RT under N2 for 12 h. After 12 h, the solvent was removed in vacuo, and the residue was diluted with 20 mL of H2O, then extracted with CHCl3/IpOH (3:1, 3×20 mL). The combined organic portions were washed with brine, and dried over MgSO4, and the solvents were removed in vacuo to yield a residue. Purification over silica gel (gradient, 5% to 7.5% MeOH/CH2Cl2 with 0.5% of TEA) provided the title compound as an off-white solid. MS m/z: 439 (M+H). Calc'd for C22H26N6O2S: 438.18.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07196104B2 |
| Source dataset | uspto-grants-2007_03 |
| ORD ID | ord-9f57f625a0484665b9de3efed9e88743 |
| Source note | uspto-grants-2007_03 |