関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | 3-((2-Amino-4-chlorophenyl)amino)propan-1-ol | HCID 3017357 | — |
| 反応物 | Potassio isocyanate | HCID 11051572 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | 5-chloro-1,3-dihydro-1-(3-hydroxypropyl)-2H-benzimidazol-2-one | HCID 3017358 | 32% |
反応手順
To a stirred solution of 40 parts of 3-[(2-amino-4-chlorophenyl)amino]-1-propanol in 140 parts of water and 24 parts of a hydrochloric acid solution 10 N is added dropwise a solution of 18 parts of potassium isocyanate in 40 parts of water (exothermic reaction: temperature rises to 35° C.). Upon completion, stirring is continued first for 30 minutes at room temperature and further for 20 hours at reflux temperature. The reaction mixture is allowed to stirr over week-end without heating. The precipitated product is filtered off and treated with a diluted hydrochloric acid solution in 4-methyl-2-pentanone. The whole is stirred and the layers are separated. The 4-methyl-2-pentanone-phase is washed with water, dried, filtered and evaporated, yielding 18 parts (32%) of 5-chloro-1,3-dihydro-1-(3-hydroxypropyl)-2H-benzimidazol-2-one; mp. 148.8° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US04175129 |
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| 出典データセット | uspto-grants-1979_11 |
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| ORD ID | ord-54013cc3ad1b41dcbaa1c75bccb9716b |
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| 出典メモ | uspto-grants-1979_11 |
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