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Potassium Carbonate → HCID 59300816、化合物
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | 3-Chloro-1-butyne | HCID 30443 | — |
| 反応物 | 1,8-Diazabicyclo(5.4.0)undec-7-ene | HCID 81184 | — |
| 反応物 | N-(3,3-Dimethyl-6-nitro-2-oxo-2,3-dihydro-1H-indol-5-yl)acetamide | HCID 23092658 | — |
| 溶媒 | Methanol | HCID 887 | — |
| 生成物 | HCID 59300816 | HCID 59300816 | 50.1% |
反応手順
Analogously to general procedure (I) N-(3,3-dimethyl-6-nitro-2-oxo-2,3-dihydro-1H-indol-5-yl)-acetamide (2.5 g) is alkylated using (rac)-3-chloro-but-1-yne (0.86 g; 9.5 mmol) and K2CO3 (3.28 g; 23.7 mmol) at 50° C. for 14 days. After aqueous work-up the crude material (1.51 g) is de-acetylated in MeOH (40 ml) using DBU (0.3 ml) at reflux. After aqueous work-up (rac)-5-amino-3,3-dimethyl-1-(1-methyl-prop-2-ynyl)-6-nitro-1,3-dihydro-indol-2-one (1,3 g) is obtained and used without further purification.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07714010B2 |
| 出典データセット | uspto-grants-2010_05 |
| ORD ID | ord-60c0f55c6f6243309cf33691b10c6972 |
| 出典メモ | uspto-grants-2010_05 |