関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Methanol | HCID 887 | — |
| 反応物 | Thionyl Chloride | HCID 24386 | — |
| 反応物 | Sodium Acetate | HCID 517045 | — |
| 反応物 | 1-(7-Chloroquinazolin-4-yl)-5-methoxy-2-methylindol-3-ylacetic acid | HCID 10194003 | — |
| 溶媒 | Ethanol | HCID 702 | — |
| 溶媒 | Chloroform | HCID 6212 | — |
| 生成物 | HCID 21449337 | HCID 21449337 | — |
反応手順
To a solution of anhydrous 1-(7-chloroquinazolin-4-yl)-5-methoxy-2-methylindol-3-ylacetic acid (1.0g.) in ethanol-free chloroform (30 ml; dried over calcium chloride) was added a solution of thionyl chloride (0.19 ml.) in chloroform (2ml). The resulting dark red solution was stirred at room temperature for 30 mins., and then methanol (20 ml.) was added. The mixture was heated under reflux for 30 mins., saturated sodium acetate solution (2 ml.) was added, and the mixture was concentrated in vacuo. Water (30 ml.) was added to the residue and the mixture was extracted with ether (3 × 30 ml.). The ether extracts were washed successively with saturated sodium hydrogen carbonate solution (30 ml.) and water (30 ml.), and dried (Na2SO4). Evaporation of the solvent gave a dark yellow oil, which slowly crystallised to give methyl 1-(7-chloroquinazolin-4-yl)-5-methoxy-2-methylindol-3-ylacetate, 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 | US04012513 |
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| 出典データセット | uspto-grants-1977_03 |
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| ORD ID | ord-9fa89b6832194ee3a953211cb7b9b4c4 |
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| 出典メモ | uspto-grants-1977_03 |
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