関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Benzyl Alcohol | HCID 244 | — |
| 反応物 | p-Toluenesulfonic acid monohydrate | HCID 521998 | — |
| 反応物 | (3-Aminophenyl)acetic acid | HCID 571807 | — |
| 反応物 | alpha-benzyl 4-[N,N-bis(2-chloroethyl)-amino]phenoxycarbonyl-gamma-(3-methylphenyl)-L-glutamine | HCID 86752016 | — |
| 溶媒 | Toluene | HCID 1140 | — |
| 生成物 | HCID 86748614 | HCID 86748614 | — |
反応手順
3-amino-phenylacetic acid benzyl ester p-toluene sulphonic acid was prepared by adding 3-aminophenylacetic acid (10 g) and p-toluene sulphonic acid monohydrate (13.2 g) to benzyl alcohol (27.2 ml) in toluene (30 ml). The mixture was heated under reflux and the water formed collected in a Dean-Stark receiver. When all the water had been distilled off the mixture was allowed to cool to 25° C. before diluting with diethyl ether and placing in an ice-bath for 1 hr. The crystalline p-toluene sulphonate was filtered off and dried in a dissicator (23.5 g) NMR δ 2.31(s)3H, 3.82(s)2H, 5.11(s)2H, 7.11(d)2H, 7.25-7.45(m)8H, 7.52(d)2H.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US06277880B1 |
|---|
| 出典データセット | uspto-grants-2001_08 |
|---|
| ORD ID | ord-39c1dfe6c3664335ba8d574c2856116d |
|---|
| 出典メモ | uspto-grants-2001_08 |
|---|
