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Sodium Carbonate → 5Bromo-4-chloro-4-fluoro-3,4,5,6-tetrahydrophthalic anhydride
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Sodium Carbonate | HCID 10340 | — |
| 反応物 | Bromine | HCID 24408 | — |
| 反応物 | Pyridine, hydrofluoride (1:1) | HCID 64774 | — |
| 反応物 | 4-Chloro-3,6-dihydrophthalic anhydride | HCID 10986977 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | 5Bromo-4-chloro-4-fluoro-3,4,5,6-tetrahydrophthalic anhydride | HCID 11098057 | — |
反応手順
Pyridinium poly(hydrogen fluoride) was added to a solution of 4-chloro-3,6-dihydrophthalic anhydride (6.5 g) in methylene chloride (10.1 g) at room temperature. Bromine (3.1 g) was added. A violent reaction occurs. The solution was allowed to stand for 6 hours and then was poured into a two phase mixture of methylene chloride (30 ml) and solid sodium carbonate. The suspension was stirred for 10 minutes until bubbling stopped. The mixture was filtered and the methylene chloride removed under reduced pressure. The material was purified by a bulb to bulb distillation (140° C. air temperature and 2.8 torr) to give a yellowish solid, (3.74 g).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05322954 |
| 出典データセット | uspto-grants-1994_06 |
| ORD ID | ord-8d4d1e2b6eb74cb0a5fd90834ca6e944 |
| 出典メモ | uspto-grants-1994_06 |