関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Benzyl Alcohol | HCID 244 | — |
| 反応物 | Diisopropylethylamine | HCID 81531 | — |
| 反応物 | P,P-Diphenylphosphinic azide | HCID 199401 | — |
| 反応物 | 3-Oxocyclobutane-1-carboxylic acid | HCID 4913358 | — |
| 溶媒 | Toluene | HCID 1140 | — |
| 生成物 | Benzyl (3-oxocyclobutyl)carbamate | HCID 19794323 | 50% |
反応手順
To a solution of 3-oxocyclobutanecarboxylic acid (1.0 g, 8.77 mmol) and DIEA (1.92 g, 14.92 mmol) in toluene (8 mL) was added DPPA (2.89 g, 10.52 mmol) at rt. The mixture was heated to 60° C. under Argon for 3 h, then benzyl alcohol (1.14 g, 10.52 mmol) was added. The mixture was stirred at 60° C. overnight. The reaction was concentrated, the residue was purified by SGC (PE:EA=8:1) to afford the desired compound (240 mg, yield 50%). 1H NMR (500 MHz, CDCl3): δH 7.38-7.33 (m, 5H), 5.12 (d, J=7.5 Hz, 2H), 4.34-4.33 (brs, 1H), 3.44-3.39 (m, 2H), 3.10-3.07 (brs, 2H) ppm; ESI-MS (m/z): 220.2 [M+1]+.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US09096634B2 |
|---|
| 出典データセット | uspto-grants-2015_08 |
|---|
| ORD ID | ord-56bdcebd2c844aebba11c53a4cf5e8a8 |
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| 出典メモ | uspto-grants-2015_08 |
|---|
