関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Acetic Anhydride | HCID 7918 | — |
| 反応物 | Compound 7189 | HCID 130176 | — |
| 溶媒 | Pyridine | HCID 1049 | — |
| 生成物 | N-acetyl-2-amino-N-methyl-alpha-(3-methyl-2-thienyl)benzeneethanamine | HCID 22414447 | 50.5% |
反応手順
A stirred, ice water chilled solution of 5.07 g of 2-amino-N-methyl-α-(3-methyl-2-thienyl)benzeneethanamine in 40 ml of pyridine was treated dropwise with 2.25 g of acetic anhydride. The solution was stirred with cooling for 15 minutes and then at room temperature for 3 hours. After standing overnight, the reaction mixture was decanted into water (200 ml), treated with dichloromethane (100 ml) and basified with 10% sodium hydroxide solution. The aqueous phase was extacted with dichloromethane (150 ml), and the combined organic phase was filtered and concentrated. The resulting solid was stirred with toluene and evaporated to dryness. Recrystallization from propionitrile (14 ml) afforded 3.0 g of N-acetyl-2-amino-N-methyl-α-(3-methyl-2-thienyl)benzeneethanamine, mp 176°-181.5° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US05292760 |
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| 出典データセット | uspto-grants-1994_03 |
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| ORD ID | ord-6904f10396fd43aba71c444b02a81509 |
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| 出典メモ | uspto-grants-1994_03 |
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