関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | Isocyanic acid | HCID 6347 | — |
| 反応物 | Alpha-Methylstyrene | HCID 7407 | — |
| 反応物 | Carbamic chloride | HCID 68048 | — |
| 反応物 | (1-Chloro-1-methylethyl)benzene | HCID 70281 | — |
| 触媒 | Zincchloride | HCID 3007855 | — |
| 溶媒 | Toluene | HCID 1140 | — |
| 溶媒 | Isobutyl ketone | HCID 7958 | — |
| 生成物 | 1-Methyl-1-phenyl-ethylisocyanate | HCID 2769430 | 75% |
反応手順
0.365 grams of dry hydrogen chloride (0.010 mole) was introduced into a solution of 0.43 grams of isocyanic acid (0.010 mole) in 3.44 grams of toluene at 0° under a nitrogen atmosphere. 1.18 gram of α-methylstyrene (0.010 mole) was added to the resultant carbamoyl chloride solution over a period of ten minutes while maintaining the temperature at 0° C. After fifteen minutes, cumyl chloride was present in 75% yield. 11.5 ml of 20.4% isocyanic acid in toluene (0.050 mole) was then added at 0° C. followed by addition of 0.50 ml of 1 M zinc chloride (0.00050 mole) in diisobutyl ketone over a period of 2 minutes at 0° C. After 5 minutes, cumyl isocyanate (b.p 50° C./1 mm was formed in 75% yield based α-methylstyrene.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US04379767 |
|---|
| 出典データセット | uspto-grants-1983_04 |
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| ORD ID | ord-4d39183e60f24986824c113eb057ed32 |
|---|
| 出典メモ | uspto-grants-1983_04 |
|---|
