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Toluene → Dichloromethane methanol ammonium hydroxide
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Toluene | HCID 1140 | — |
| 反応物 | Dichloromethane | HCID 6344 | — |
| 反応物 | Ethyl oxoacetate | HCID 70211 | — |
| 反応物 | Sodium triacetoxyborohydride | HCID 5049666 | — |
| 反応物 | N-(1,3-benzodioxol-5-ylmethyl)-N-methyl-1,3-propanediamine | HCID 22488891 | — |
| 生成物 | Dichloromethane methanol ammonium hydroxide | HCID 21896990 | — |
| 生成物 | 2-[[3-[(1,3-Benzodioxol-5-ylmethyl)amino]propyl]amino]acetic acid ethyl ester | HCID 69742407 | — |
反応手順
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)
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06670473B2 |
| 出典データセット | uspto-grants-2003_12 |
| ORD ID | ord-55108abb899d4b6da727c78b3e27185b |
| 出典メモ | uspto-grants-2003_12 |