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N,N,2,2-Tetramethylpropane-1,3-diamine → HCID 178446432、化合物
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | N,N,2,2-Tetramethylpropane-1,3-diamine | HCID 104477 | — |
| 反応物 | Benzyltriethylammonium permanganate | HCID 11781896 | — |
| 反応物 | N-(4-benzyloxyphenyl)-N'-(3-methylbutyl)thiourea | HCID 86091663 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | HCID 178446432 | HCID 178446432 | 25.9% |
反応手順
Benzyltriethylammonium permanganate (0.281 g; 1.5 eq.) is added, at 5° C. and portionwise, to a solution of N-(4-benzyloxyphenyl)-N′-(3-methylbutyl)thiourea (0.200 g) and 3-dimethylamino-2,2-dimethylpropylamine (0.156 g; 2 eq.) in tetrahydrofuran (THF; 2.2 ml). The reaction medium is stirred for three days at room temperature. After filtration and concentration, the product is purified by chromatography on silica (eluent: methanol +0.1% acetic acid). The product, dissolved in dichloromethane, is washed with 1N sodium hydroxide. After drying and concentration, 0.067 g of N-(4-benzyloxyphenyl)-N′-(3-dimethylamino-2,2-dimethylpropyl)-N″-(3-methylbutyl)guanidine is obtained.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07582656B2 |
| 出典データセット | uspto-grants-2009_09 |
| ORD ID | ord-ae43a2fc7011427a893068ca93484117 |
| 出典メモ | uspto-grants-2009_09 |