HuagongsheHuagongshe Chemistry Print Report · For research reference only
HCID 22640029, compound → HCID 22640042, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | HCID 22640029 | HCID 22640029 | — |
| Reactant | HCID 178418361 | HCID 178418361 | — |
| Solvent | Acetic Acid | HCID 176 | — |
| Solvent | Methanol | HCID 887 | — |
| Product | HCID 22640042 | HCID 22640042 | — |
Reaction Steps
A solution of 2.0 g (4.7 mmol) of (4-benzyloxy-3-cyclopropylmethoxybenzyl)(5-chloro-2,6-dimethyl-pyrimidin-4-yl)amine (from example A5) in 50 ml of methanol and 20 ml of glacial acetic acid is admixed with 250 mg of Pd-on-carbon catalyst (type 38H, Johnson Matthey) and hydrogenated by circulation with hydrogen until about 2 equivalents of hydrogen (about 350 ml) have been taken up. After filtration to remove the catalyst, the solution is concentrated and the residue is chromatographed on silica gel (mobile phase: toluene/dioxane/ammonia=2:1:0.05). The fractions with Rf=0.15 are collected and concentrated. The residue (1.5 g), which is of poor solubility, is reacted further without additional purification (see example 7).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06818642B2 |
| Source dataset | uspto-grants-2004_11 |
| ORD ID | ord-7c845ae89dc044f8bbb79d17e6a17bc8 |
| Source note | uspto-grants-2004_11 |