関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Morpholine | HCID 8083 | — |
| 反応物 | Binap, (A+-)- | HCID 634876 | — |
| 反応物 | Methyl 2-(3-bromophenyl)acetate | HCID 11746402 | — |
| 触媒 | Bis(dibenzylideneacetone)palladium | HCID 9811564 | — |
| 溶媒 | Toluene | HCID 1140 | — |
| 溶媒 | Diethyl Ether | HCID 3283 | — |
| 生成物 | Methyl 3-(morpholin-4-yl)phenylacetate | HCID 18403524 | 23% |
反応手順
A round bottom flasked flushed with argon was charged with methyl 3-bromophenyl-acetate (2.29 g, 10 mmol) (prepared from 3-bromophenylacetic acid as described in example 2, step 1), morpholine (1.05 mL, 1.2 eq.), CsCO3 (4.55 g, 1.4 eq.), Pd2(dba)3 (92 mg, 0.01 eq) and BINAP (93 mg, 0.15 eq.) in toluene (20 mL). The resulting mixture was heated at 100° C. overnight and then diluted with diethyl ether (120 mL). The precipitates were filtered through a Celite pad and the filtrate was concentrated and purified on a silica-gel column with 20% EtOAc in hexane to give methyl 3-(morpholin-4-yl)phenylacetate (0.55 g, 23%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US06479490B2 |
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| 出典データセット | uspto-grants-2002_11 |
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| ORD ID | ord-d77f8454ac2a429885df267293caef92 |
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| 出典メモ | uspto-grants-2002_11 |
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