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Benzeneacetic acid, alpha-bromo-, methyl ester → 5-n-Butyl-2-[alpha-(carbomethoxy)benzyl]-2,4-dihydro-4-[[2'-(N-trityltetrazol-5-yl)biphenyl-4-yl]methyl]-3H-1,2,4-triazol-3-one
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Benzeneacetic acid, alpha-bromo-, methyl ester | HCID 137806 | — |
| 反応物 | 5-n-Butyl-2,4-dihydro-4-[[2'-(N-trityltetrazol-5-yl)biphenyl-4-yl]methyl]-3H-1,2,4-triazol-3-one | HCID 19939386 | — |
| 生成物 | 5-n-Butyl-2-[alpha-(carbomethoxy)benzyl]-2,4-dihydro-4-[[2'-(N-trityltetrazol-5-yl)biphenyl-4-yl]methyl]-3H-1,2,4-triazol-3-one | HCID 19939404 | 57% |
反応手順
The alkylation of 5-n-butyl-2,4-dihydro-4-[[2'-(N-trityltetrazol-5-yl)biphenyl-4-yl]methyl]-3H-1,2,4-triazol-3-one (from Example 2, Step D) with methyl α-bromophenyl-acetate was carried out as described in Example 3, Step A, except 3 equivalents of the alkylating agent was used. After work-up, flash chromatography of the crude product over silica gel (50 mL for 0.24 mmole, elution with 0.5% MeOH/CH2Cl2) gave the title compound in 57% yield as an oil, homogeneous by TLC in 2% MeOH/CH2Cl2, mass spectrum (FAB) m/e 766 (M+1)+.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05411980 |
| 出典データセット | uspto-grants-1995_05 |
| ORD ID | ord-498e6b5eba2c43d4a957517d7cb0c428 |
| 出典メモ | uspto-grants-1995_05 |