関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | Diazomethane | HCID 9550 | — |
| 反応物 | Isobutyl chloroformate | HCID 62365 | — |
| 反応物 | 2-(4-chloro-N-(pent-1-yn-3-yl)phenylsulfonamido)-butanoic acid | HCID 59342373 | — |
| 溶媒 | Acetic Acid | HCID 176 | — |
| 溶媒 | Diethyl Ether | HCID 3283 | — |
| 生成物 | 4-chloro-N-(1-diazo-2-oxopentan-3-yl)-N-(pent-1-yn-3-yl)benzenesulfonamide | HCID 72259587 | — |
反応手順
To a solution of the compound 60 (498 mg, 1.45 mmol) in 7.5 mL of Et2O were added sequentially 0.24 mL of triethylamine (1.2 eq), 0.23 mL of isobutyl chloroformate (1.2 eq) at −30° C. After being stirred at −30° C. for 15 min, diazomethane (prepared by mixing MNNG and KOH in diethyl ether) (excess) was added to the above mixture at 0° C. and stirred there for 5 hours. Glacial HOAc (1.5 mL) was added to destroy the excess diazomethane and the solution was extracted with EtOAc. The organic phase was washed with sat NaHCO3, water, brine and dried (MgSO4). LCMS 368.1 (M+1).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US07732609B2 |
|---|
| 出典データセット | uspto-grants-2010_06 |
|---|
| ORD ID | ord-c6a04bb7504c4ce18d8cc8e65ca5dd39 |
|---|
| 出典メモ | uspto-grants-2010_06 |
|---|