関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Isobutyric Acid | HCID 6590 | — |
| 反応物 | Trimethyl orthoacetate | HCID 15050 | — |
| 反応物 | 1,1,1-Trifluoro-2-bromo-2-chloro-5-methyl-4-hexen-3-ol | HCID 15219346 | — |
| 生成物 | 5-Bromo-5-chloro-4-(1,1-dimethoxyethoxy)-2-methyl-6,6,6-trifluorohex-2-ene | HCID 15278702 | — |
反応手順
5-Bromo-5-chloro-4-hydroxy-2-methyl-6,6,6-trifluorohex-2-ene (10.0 g), trimethyl orthoacetate (48.0 g) and isobutyric acid (0.29 g) were charged to a round-bottomed flask fitted with: nitrogen inlet/bubbler, thermometer and Dean and Stark received packed with 5A molecular seives. The mixture was heated with agitation to reflux and distillates collected until reaction mass temperature increased to 111° C. (ca. 1 hr). Once the reaction was complete, the residual trimethyl orthoacetate was removed by distillation under vacuum (ca. 50° C. @ 50 mmHg) to give the product, 5-bromo-5-chloro-4-(1,1-dimethoxyethoxy)-2-methyl-6,6,6-trifluorohex-2-ene, as an orange oil (10.9 g, 85% yield).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US05731475 |
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| 出典データセット | uspto-grants-1998_03 |
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| ORD ID | ord-5232ccbb96cf4bf19ed922c74f60ad33 |
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| 出典メモ | uspto-grants-1998_03 |
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