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Acrylic Acid → HCID 10523147、化合物
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Acrylic Acid | HCID 6581 | — |
| 反応物 | 1,3-Propanediamine, N'-(ethylcarbonimidoyl)-N,N-dimethyl-, monohydrochloride | HCID 2723939 | — |
| 反応物 | 4-N-(3-bromophenyl)pyrido[3,2-d]pyrimidine-4,6-diamine | HCID 5328274 | — |
| 反応物 | Dichloromethane ethylacetate | HCID 21226138 | — |
| 溶媒 | Dimethylacetamide | HCID 31374 | — |
| 溶媒 | Methylenechloride Hexane | HCID 21226440 | — |
| 溶媒 | Dichloromethane ethyl acetate methanol | HCID 21901258 | — |
| 生成物 | HCID 10523147 | HCID 10523147 | 26% |
反応手順
To a stirred solution of 6-amino-4-[(3-bromo-phenyl)amino]pyrido[3,2-d]pyrimidine (J Med Chem, 1996;39:1823) (46 mg, 0.15 mmol) and acrylic acid (6 mol eq., 0.91 mmol, 62 μL) in DMA (5.0 mL) under N2 was added 1-(3-dimethylaminopropyl)-3-ethylcarbodiimide hydrochloride (EDCI.HCl) (4.0 mol eq., 0.61 mmol, 116 mg). The reaction mixture was stirred for 48 hours with additional amounts of acrylic acid and EDCI.HCl (62 μL/116 mg) being added every 12 hours it was then worked up as above to give after chromatography on silica gel eluting with EtOAc:CH2Cl2 (1:1) to MeOH/CH2Cl2/EtOAc (2:48:50), N-[4-[(3-bromophenyl)-amino]pyrido[3,2 -d]pyrimidin-6-yl]acrylamide (14 mg, 26%) as a cream powder, mp (CH2Cl2/hexane) 226-228° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06602863B1 |
| 出典データセット | uspto-grants-2003_08 |
| ORD ID | ord-74e3ef88c60b4122bd3f1a50ca0f92b0 |
| 出典メモ | uspto-grants-2003_08 |