HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Toluene → Dichloromethane methanol ammonium hydroxide
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Toluene | HCID 1140 | — |
| Edukt | Dichloromethane | HCID 6344 | — |
| Edukt | Ethyl oxoacetate | HCID 70211 | — |
| Edukt | Sodium triacetoxyborohydride | HCID 5049666 | — |
| Edukt | N-(1,3-benzodioxol-5-ylmethyl)-N-methyl-1,3-propanediamine | HCID 22488891 | — |
| Produkt | Dichloromethane methanol ammonium hydroxide | HCID 21896990 | — |
| Produkt | 2-[[3-[(1,3-Benzodioxol-5-ylmethyl)amino]propyl]amino]acetic acid ethyl ester | HCID 69742407 | — |
Reaktionsschritte
To N-(1,3-benzodioxol-5-ylmethyl)-N-methyl-1,3-propanediamine (33 g, 0.15 mol) in CH2Cl2 (500 mL) was added ethyl glyoxalate (30 mL of a 50% toluene solution, 0.15 mol) and sodium triacetoxyborohydride (40 g, 0.19 mol). After stirring for 4 hours, the reaction was washed with aqueous potassium carbonate and the solvent removed in vacuo. Chromatography on silica with CH2Cl2/MeOH/ammonium hydroxide gave 14 g of 2-([3-[(1,3-benzodioxol-5-ylmethyl)amino]propyl]amino]acetic acid, ethyl ester, a compound of formula (Y10)
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US06670473B2 |
| Quelldatensatz | uspto-grants-2003_12 |
| ORD ID | ord-55108abb899d4b6da727c78b3e27185b |
| Quellennotiz | uspto-grants-2003_12 |