関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | Sodium hydride | HCID 24758 | — |
| 反応物 | 2-Chloro-4-phenylquinazoline | HCID 3123582 | — |
| 反応物 | 21810-34-4 | HCID 23712826 | — |
| 溶媒 | Acetic Acid | HCID 176 | — |
| 溶媒 | Sulfolaneat | HCID 86748276 | — |
| 生成物 | 6-(4-Phenyl-2-quinazolinyloxy)hexanoic acid | HCID 18987243 | 11.6% |
反応手順
To a suspension of 1.74 g of potassium 6-hydroxyhexanoate (prepared from e-caprolactone) in 35 cc of sulfolaneat 60° C. was added 0.64 g of sodium hydride (55% w/w dispersion in mineral oil). The mixture was stirred for 30 minutes to 140° C. until effervescence had stopped. 3 g of 2-chloro-4-phenyl-quinazoline were then added and the resultant mixture was heated for further 2 hours to 140° C. The mixture was poured into 500 cc of water, neutralized with acetic acid and extracted with dichloromethane (3#300 cc). The combined extracts were washed with water, dried (Na2SO4) and evaporated. The residue was chromatographed on silica gel (50-200 mm; eluent: 95:5 diethyl ether/methanol), then washed with n-hexane and filtered to give 0.4 g (10%) of 6-(4-phenyl-2-quinazolinyloxy)hexanoic acid as a whitish solid. (m.p.=112°-114° C.)
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US05366982 |
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| 出典データセット | uspto-grants-1994_11 |
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| ORD ID | ord-bf7b31a3973e4686801e6fa7dab205dc |
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| 出典メモ | uspto-grants-1994_11 |
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