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1,2-Dichloroethane → 4-Ethynylbenzoyl-2(S)-phenylsulfonylamino-beta-alanine ethyl ester
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 1,2-Dichloroethane | HCID 11 | — |
| 反応物 | 4-Methylmorpholine | HCID 7972 | — |
| 反応物 | 1-Hydroxybenzotriazole | HCID 75771 | — |
| 反応物 | 4-Ethynylbenzoic acid | HCID 589706 | — |
| 反応物 | Ethyl 2(S)-phenylsulfonylamino-beta-alanine p-toluenesulfonate | HCID 86752459 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | 4-Ethynylbenzoyl-2(S)-phenylsulfonylamino-beta-alanine ethyl ester | HCID 86752458 | — |
反応手順
4-Ethynylbenzoic acid (35-1) (3.10 g, 21.2 mmol), 35-2 (8.58 g, 19.3 mmol), NMM (8.49 mL, 7.72 mmol), HOBT (3.39 g, 25.1 mmol), and EDC (4.81 g, 25.1 mmol) were combined in 96 mL DMF and stirred overnight. The reaction was concentrated, residue was diluted with EtOAc and washed with water (2×) and brine, dried (Na2SO4), filtered, and concentrated. Flash chromatography (silica, 45-50% EtOAc/Hexane) gave 35-3 as a white solid.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05929120 |
| 出典データセット | uspto-grants-1999_07 |
| ORD ID | ord-268a8eabed7640b0a9ec915cc4429c22 |
| 出典メモ | uspto-grants-1999_07 |