HuagongsheHuagongshe Chemistry Print Report · For research reference only
Water → HCID 136069591, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Water | HCID 962 | — |
| Reactant | Dichloromethane | HCID 6344 | — |
| Reactant | Chlorosuccinimide | HCID 31398 | — |
| Reactant | Ethyl 2-[4-(morpholin-4-yl)-6-oxo-1,6-dihydropyrimidin-2-yl]acetate | HCID 135905419 | — |
| Solvent | Chloroform | HCID 6212 | — |
| Product | HCID 136069591 | HCID 136069591 | 66.5% |
Reaction Steps
1.87 g of N-chlorosuccinimide are added to a solution of 3.75 g of ethyl [4-(morpholin-4-yl)-6-oxo-1,6-dihydropyrimidin-2-yl]acetate described in example 6a (step (2′a)a) in 50 ml of chloroform. The reaction medium is stirred at ambient temperature for 2 hours. 20 ml of water and 50 ml of dichloromethane are added. After settling out, the organic phase is dried over magnesium sulfate, filtered, and then concentrated under reduced pressure. The residue obtained is purified on a silica column, eluent: 99/01 then 98/02 then 97/03 dichloromethane/methanol, so as to give 2.81 g of (5-chloro-4-morpholin-4-yl-6-oxo-1,6-dihydropyrimidin-2-yl)acetic acid ethyl ester, the characteristics of which are the following:
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09133168B2 |
| Source dataset | uspto-grants-2015_09 |
| ORD ID | ord-e5d3ff65d0564f3da7939164b876fa65 |
| Source note | uspto-grants-2015_09 |