HuagongsheHuagongshe Chemistry Print Report · For research reference only
1,2-Dichloroethane → HCID 178473393, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | 1,2-Dichloroethane | HCID 11 | — |
| Reactant | 1-Hydroxybenzotriazole | HCID 75771 | — |
| Reactant | HCID 66856328 | HCID 66856328 | — |
| Reactant | HCID 178418698 | HCID 178418698 | — |
| Solvent | Water | HCID 962 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | HCID 178473393 | HCID 178473393 | — |
Reaction Steps
To a solution of 1 g of 4-Hydroxy-7-methyl-quinoline-2-carboxylic acid and 1.7 g of 4-((S)-2-Amino-4-benzyloxy-butyryl)-piperazine-1-carboxylic acid ethyl ester trifluoroacetate in 15 ml of DMF, 566 mg of NEM, 753 mg of HOBT and 943 mg of EDC was added and the reaction mixture was stirred for 16 h at RT. Then, the reaction mixture was diluted with water and extracted with ethyl acetate. The organic phase was dried over MgSO4 and the solvents were removed under reduced pressure. The crude product was precipitated from a mixture of n-heptane and ethyl acetate. The precipitated product was collected by filtration and dried under reduced pressure. The isolated product was pure enough for the next reaction step. Yield: 1.8 g.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08669266B2 |
| Source dataset | uspto-grants-2014_03 |
| ORD ID | ord-e0cfc69f45cf4bf9a6c79baedc550eea |
| Source note | uspto-grants-2014_03 |