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1,2-Phenylenediamine dihydrochloride → 3-(1H-benzimidazol-2-yl)-butan-1-ol
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 1,2-Phenylenediamine dihydrochloride | HCID 11990 | — |
| 反応物 | alpha-Methylbutyrolactone | HCID 98323 | — |
| 溶媒 | Hydrochloric Acid | HCID 313 | — |
| 生成物 | 3-(1H-benzimidazol-2-yl)-butan-1-ol | HCID 18407015 | 126.9% |
反応手順
Following the general procedure described in A. R. Friedman, D. S. Payne and A. R. Day, J. Heterocyclic Chemistry, 3:257-259(1966), a mixture of 9 g of 1,2-phenylenediamine dihydrochloride and 7 g of 2-methylbutyrolactone in 60 mL of 4N hydrochloric acid was heated to reflux for 4 days, 1 teaspoon of decolorizing carbon added, and after another 15 min reflux, filtered hot. The filtrate was concentrated under reduced pressure to near dryness, the residue made basic (pH=8) with ammonium hydroxide and extracted into 3×100 mL of ethyl acetate. The combined extracts were dried over magnesium sulfate and concentrated under reduced pressure. After drying under vacuum, 12 g of 3-(1H-benzimidazol-2-yl)-butan-1-ol was obtained as a resin.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06476041B1 |
| 出典データセット | uspto-grants-2002_11 |
| ORD ID | ord-c3402856b1b044e9a112a35d3f7211ca |
| 出典メモ | uspto-grants-2002_11 |