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Water → 4-(4-tert-Butylbenzoylamino)isophthalic acid
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | 4-tert-Butylbenzoyl chloride | HCID 74372 | — |
| 反応物 | 4-Aminobenzene-1,3-dioic acid | HCID 11355852 | — |
| 溶媒 | Acetone | HCID 180 | — |
| 生成物 | 4-(4-tert-Butylbenzoylamino)isophthalic acid | HCID 21906414 | 29% |
反応手順
Into 60 mL acetone was dissolved 0.905 g (5 mmol) 4-aminoisophthalic acid. To the solution was added 30 mL water. The mixture was cooled in an ice bath, and 1.08 mL (5.5 mmol) 4-tert-butylbenzoyl chloride in 10 mL acetone was added dropwise. The mixture was allowed to warm slowlyly to room temperature and after 24 h was concentrated under vacuum and shaken between EtOAc (150 mL) and cold dilute HCl (150 mL). The organic layer was dried (MgSO4) and evaporated. The desired crystalline product (0.489 g, 29%) was obtained from methylene chloride-hexane.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07129245B2 |
| 出典データセット | uspto-grants-2006_10 |
| ORD ID | ord-9ca1d60fb6c443faac0c4569fa720387 |
| 出典メモ | uspto-grants-2006_10 |