HuagongsheHuagongshe Chemistry Print Report · For research reference only
1,1-Dimethoxyethyl(dimethyl)amine → N'-[(6S)-2-(3-Chloro-4-fluorobenzyl)-10-methoxy-8-ethyl-6-methyl-1,9-dioxo-1,2,6,7,8,9-hexahydropyrazino[1',2':1,5]pyrrolo[2,3-d]pyridazin-4-yl]-N,N-dimethylethanimidamide
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | 1,1-Dimethoxyethyl(dimethyl)amine | HCID 87835 | — |
| Reactant | (6S)-4-Amino-2-(3-chloro-4-fluorobenzyl)-10-methoxy-8-ethyl-6-methyl-7,8-dihydropyrazino[1',2':1,5]pyrrolo[2,3-d]pyridazine-1,9(2H,6H)-dione | HCID 68865350 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | N'-[(6S)-2-(3-Chloro-4-fluorobenzyl)-10-methoxy-8-ethyl-6-methyl-1,9-dioxo-1,2,6,7,8,9-hexahydropyrazino[1',2':1,5]pyrrolo[2,3-d]pyridazin-4-yl]-N,N-dimethylethanimidamide | HCID 68865133 | — |
Reaction Steps
A solution of (6S)-4-amino-2-(3-chloro-4-fluorobenzyl)-10-methoxy-8-ethyl-6-methyl-7,8-dihydropyrazino[1′,2′:1,5]pyrrolo[2,3-d]pyridazine-1,9(2H,6H)-dione (0.20 g, 0.46 mmol; Example 120, step 3) and N,N-dimethylacetamide dimethyl acetal (0.37 mL, 2.51 mmol) in anhydrous DMF (50 mL) was stirred in an oil bath at 40° C. overnight. The reaction mixture was concentrated under vacuum. The residue was subjected to column chromatography on silica gel eluting with a 0-5% methanol in chloroform gradient. Collection and concentration of appropriate fractions provided the title compound.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07538112B2 |
| Source dataset | uspto-grants-2009_05 |
| ORD ID | ord-20e06b25089c494fa34aa358c33081b6 |
| Source note | uspto-grants-2009_05 |