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4-Methyl-5-(2-hydroxyethyl)thiazole → HCID 21299287、化合物
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 4-Methyl-5-(2-hydroxyethyl)thiazole | HCID 1136 | — |
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | Acryloyl chloride | HCID 13140 | — |
| 触媒 | Phenothiazine | HCID 7108 | — |
| 溶媒 | Chloroform | HCID 6212 | — |
| 生成物 | HCID 21299287 | HCID 21299287 | 82% |
反応手順
A one liter, three necked flask was equipped with overhead stirrer, nitrogen atmosphere and an addition funnel. The flask was charged with 100 g of 5-(2-hydroxyethyl)-4-methylthiazole (0.70 mol.), 71 g of triethylamine (0.70 mol.), 500 g of chloroform and 3 g of phenothiazine. Next, 63 g of acryloyl chloride (0.70 mol.) was slowly added to the reaction over 1.5 hour via the addition funnel. The reaction was stirred for 2 hours at room temperature. The reaction mixture was extracted with NaCl(aq.), NH4OH(10%), NaCl(aq.) and dried over MgSO4. The chloroform was evaporated with a rotoevaporator to yield 113 g (82%) of a dark brown liquid. The product was confirmed by IR and 13C NMR.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05523152 |
| 出典データセット | uspto-grants-1996_06 |
| ORD ID | ord-8627cfb12c4d4690b5b4114f3be7f363 |
| 出典メモ | uspto-grants-1996_06 |