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Hydrochloric Acid → N-Trifluoroacetyl 4-benzoylphenylalanine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | Methyl trifluoroacetate | HCID 9893 | — |
| 反応物 | p-benzoyl-L-phenylalanine | HCID 7020128 | — |
| 溶媒 | Methanol | HCID 887 | — |
| 溶媒 | Ethyl Acetate | HCID 8857 | — |
| 生成物 | N-Trifluoroacetyl 4-benzoylphenylalanine | HCID 86605421 | 18.3% |
反応手順
Methyl trifluoroacetate (89.6 μL, 891 μmoles) and triethylamine (104 μL, 743 μmoles) were added to a suspension of 4-benzoylphenylalanine (200 mg, 743 μmoles) in methanol (0.5 mL). The reaction was stirred vigorously for 24 h and then acidified with 1 N HCl until a pH of 2 was obtained. The mixture was added to ethyl acetate (10 mL), washed with 1 N HCl (2×10 mL), dried over MgSO4, and concentrated in vacuo to yield a white solid (49.7 mg, 136 μmoles, 18%). LRMS: not performed. 1H NMR: spectrum is consistent with the predicted structure.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US09440988B2 |
| 出典データセット | uspto-grants-2016_09 |
| ORD ID | ord-6cfc746f1bdc4465b4d61035638b7a27 |
| 出典メモ | uspto-grants-2016_09 |