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Hydrochloric Acid → HCID 10103612、化合物
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | 2-Hexanone | HCID 11583 | — |
| 反応物 | Sodium amide | HCID 24533 | — |
| 反応物 | Methyl methoxyacetate | HCID 80507 | — |
| 溶媒 | Diethyl Ether | HCID 3283 | — |
| 生成物 | HCID 10103612 | HCID 10103612 | 122.6% |
反応手順
2-Hexanone (96.8 g) was added dropwise over 15 min under nitrogen to a stirred suspension of sodium amide (37.7 g) in dry ether (1 liter) at room temperature. The mixture was stirred for 12 min, a solution of methyl methoxyacetate (50.3 g) in dry ether (150 ml) was added dropwise over 20 min, and the mixture was heated under reflux for 2 h. The mixture was cooled, poured into ice and 2N hydrochloric acid (600 ml) and the aqueous layer extracted with ether (4×300 ml). The organic layers were washed with 8% sodium bicarbonate solution and brine, dried and evaporated to give an orange liquid (102 g). Purification by DFC, eluting with System A (5:95) gave a yellow liquid (36 g).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05389659 |
| 出典データセット | uspto-grants-1995_02 |
| ORD ID | ord-694a9480f5a84dfb9d79b562632804fb |
| 出典メモ | uspto-grants-1995_02 |