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2,6-Dichlorobenzoyl chloride → n-(2,6-Dichlorobenzoyl)-d-tyrosine methyl ester
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 2,6-Dichlorobenzoyl chloride | HCID 78392 | — |
| 反応物 | Diisopropylethylamine | HCID 81531 | — |
| 反応物 | methyl D-tyrosinate hydrochloride | HCID 134565 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | n-(2,6-Dichlorobenzoyl)-d-tyrosine methyl ester | HCID 54468447 | — |
反応手順
A solution of 2,6-dichlorobenzoylchloride (0.68 mL) in CH2Cl2 (5 mL) was added to a solution of an ice-cold solution of D-tyrosine methyl ester HCl salt (1.0 g) and DIEA (2.26 mL) in CH2Cl2 (15 mL). The mixture was stirred at room temperature for 24 h. The mixture was diluted with CH2Cl2 (50 mL) and washed successively with H2O, 1 N HCl and brine. The organic layer was dried (MgSO4) and evaporated, and the residue was recrystallized from EtOAc and hexanes to yield 1.46 g of N-(2,6-dichlorobenzoyl)-D-tyrosine methyl ester. ESMS: m/z 369 (MH+).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06855843B2 |
| 出典データセット | uspto-grants-2005_02 |
| ORD ID | ord-bcaf08c5d8d649d39fd05e7a41426600 |
| 出典メモ | uspto-grants-2005_02 |