Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | DL-alanine | HCID 602 | — |
| Reactant | Methanesulfonic Acid | HCID 6395 | — |
| Reactant | HCID 54473406 | HCID 54473406 | — |
| Solvent | 2,2,2-Trifluoroethanol | HCID 6409 | — |
| Product | HCID 53696734 | HCID 53696734 | 58.1% |
Reaction Steps
Preparation of 2-amino-propionic acid 4-(2-{3-[5-(2,4-diamino-pyrimidin-5-ylmethyl)-2,3-dimethoxy-phenyl -acryloyl}-1,2-dihydro-phthalazin-1-yl)-benzyl ester ##STR16## A solution of 130 mg of 2-tert-butoxycarbonylamino-propionic acid 4-(2-(3-[5-(2,4-diamino-pyrimidin-5-ylmethyl)-2,3-dimethoxy-phenyl]-acryloyl)-1,2-dihydro-phthalazin-1-yl)-benzyl ester in 20 ml of trifluoroethanol is treated with 18 μl of methanesulphonic acid at room temperature over one hour. The reaction solution is concentrated, the residue is taken up in ethyl acetate and filtered. The crystals are dissolved in 5 ml of water and treated with 20 ml of pH 7 buffer. The suspension obtained is suction filtered. There are obtained 65 mg of 2-amino-propionic acid 4-(2-{3-[5-(2,4-diamino-pyrimidin-5-ylmethyl)-2,3-dimethoxy-phenyl]-acryloyl)-1,2-dihydro-phthalazin-1-yl)-benzyl ester, MS (ISP): 622.3 (M+H)+
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US06114330 |
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| Source dataset | uspto-grants-2000_09 |
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| ORD ID | ord-1a1cf166463f41d0958fe6d6d6f8dfaf |
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| Source note | uspto-grants-2000_09 |
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