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Hydrochloric Acid → N-(trifluoroacetyl)aminoacetic acid
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | Glycine | HCID 750 | — |
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | Methyl trifluoroacetate | HCID 9893 | — |
| 溶媒 | Methanol | HCID 887 | — |
| 溶媒 | Ethyl Acetate | HCID 8857 | — |
| 生成物 | N-(trifluoroacetyl)aminoacetic acid | HCID 136227 | 87% |
反応手順
Methyl trifluoroacetate (804 μL, 7.99 mmoles) and triethylamine (928 μL, 6.66 mmoles) were added to a suspension of glycine (500 mg, 6.66 mmoles) in methanol (2.5 mL). After the mixture was stirred vigorously for 18 h, 1 N HCl was added dropwise until the a pH of 2 was obtained. The reaction was added to ethyl acetate (30 mL) was washed with 1 N HCl (2×10 mL), dried over MgSO4, and concentrated in vacuo to yield the amide as a white solid (991 mg, 5.79 mmoles, 87%). LRMS: (CI+) calcd for C4H4NO3F3 (M+NH4): 189; found: 189. 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 | US07098196B1 |
| 出典データセット | uspto-grants-2006_08 |
| ORD ID | ord-2b7d1cffff564c4a9cb1d06f37c1aa66 |
| 出典メモ | uspto-grants-2006_08 |