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Benzenecarboximidic acid, ethyl ester, hydrochloride (1:1) → HCID 178495957、化合物
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Benzenecarboximidic acid, ethyl ester, hydrochloride (1:1) | HCID 79249 | — |
| 反応物 | Aminoacetaldehyde dimethyl acetal | HCID 89728 | — |
| 溶媒 | Methanol | HCID 887 | — |
| 溶媒 | Sodium Hydroxide | HCID 14798 | — |
| 生成物 | HCID 178495957 | HCID 178495957 | 104.5% |
反応手順
(EX-1A) A solution of ethyl benzimidate hydrochloride (92.25 g, 496.9 mmol) in 300.0 mL dry methanol (1.68 M) was cooled to ca 0° C. and added a solution of aminoacetaldehyde dimethyl acetal (73.10 mL, 670.9 mmol) in dry methanol (75.0 mL, 9.0 M) drop wise at such a rate the temperature was kept below 5° C. The resulting solution was allowed to stir for 3 days with the temperature being maintained below 5° C. The reaction mixture was then concentrated under reduced pressure to give a yellow oil. The residue was dissolved in 1 N NaOH (750 mL) and extracted with dichloromethane (4×250 mL). The organic solutions were combined, dried (MgSO4), and concentrated to give 108.13 g crude N-(2,2-dimethoxyethyl)benzamidine as a yellow oil.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06653316B1 |
| 出典データセット | uspto-grants-2003_11 |
| ORD ID | ord-78f178215a04427989c0b929f2bacbeb |
| 出典メモ | uspto-grants-2003_11 |