関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Nitrogen | HCID 947 | — |
| 反応物 | Phosgene | HCID 6371 | — |
| 反応物 | Mandelonitrile | HCID 10758 | — |
| 溶媒 | Toluene | HCID 1140 | — |
| 生成物 | 2-Chloro-2-phenylacetonitrile | HCID 12376317 | 967.2% |
反応手順
150 g of toluene and 7 g (0.02 mol) of Cyanex® 923 are initially introduced into a phosgenation apparatus with attached carbonic acid condenser and heated. At 99° C., 13 g of phosgene are gassed in over the course of 10 minutes. Thereafter, over the course of 2 hours, 192 g (1.44 mol) of benzaldehyde cyanohydrin and a further 149 g (total=172 g or 1.74 mol) of phosgene are added in parallel. The internal temperature is maintained between 99 and 102° C. throughout. After a post-reaction of 60 minutes at 99° C., excess phosgene is stripped out using N2 at 50° C. for 2.5 h. The discharge of 359 g is fractionally distilled on a 30 cm Vigreux column. The main fraction passes over at 0.6 mbar and a head temperature of from 68 to 73° C. 192.7 g (88.3% of theory) of α-chlorophenylacetonitrile are isolated.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US06353127B1 |
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| 出典データセット | uspto-grants-2002_03 |
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| ORD ID | ord-e7f51422316643b2bba09bd562315cb9 |
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| 出典メモ | uspto-grants-2002_03 |
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