Cat.NO.:A774383 Purity:97%
Product Details of [ 101250-48-0 ]
| CAS No. : | 101250-48-0 |
| Formula : |
C11H13NO2 |
| M.W : |
191.23
|
| SMILES Code : | O=C1N[C@@H](CC2=CC=CC=C2)COC1 |
| MDL No. : | MFCD27940847 |
| InChI Key : | PXPFDUZBGQDAEP-JTQLQIEISA-N |
| Pubchem ID : | 10607734 |
Safety of [ 101250-48-0 ]
| GHS Pictogram: |  |
| Signal Word: | Warning |
| Hazard Statements: | H315-H319 |
| Precautionary Statements: | P264-P280-P302+P352-P337+P313-P305+P351+P338-P362+P364-P332+P313 |
Application In Synthesis of [ 101250-48-0 ]
* All experimental methods are cited from the reference, please refer to the original source for details. We do not guarantee the accuracy of the content in the reference.
- Downstream synthetic route of [ 101250-48-0 ]
[ 101250-48-0 ] Synthesis Path-Downstream 1~1
- 1
[ 101250-48-0 ]
[ 122-51-0 ]- [ 100-63-0 ]
[ 464174-87-6 ]
| Yield | Reaction Conditions | Operation in experiment |
|---|---|---|
| 29% | To a solution of lactam (400 mg, 2.09 mmol) in CH2Cl2 (12 mL) was added trimethyloxonium tetrafluoroborate (337 mg, 2.28 mmol) and the mixture was stirred for 16 h. To the mixture was then added phenylhydrazine (0.206 mL, 2.09 mmol) and the mixture was stirred for 20 h. The mixture was then concentrated in vacuo and redissolved in MeOH (1.5 mL) and triethyl orthoformate (4.5 mL). The mixture was heated at reflux (110 C) for 16 h then cooled to ambient temperature, whereby the product had precipitated.† The product was collected by filtration and washed with cold (-78 C) EtOAc (5 mL) to afford the title product 47 as a pale peach solid (230 mg, 29%); mp 190-195 C; inlMMLBox (c 0.8, MeOH); δH (400 MHz, DMSO-d6) 10.91 (1H, s, NCHN), 7.90-7.88 (2H, m, PhH), 7.76-7.71 (2H, m, PhH), 7.71-7.65 (1H, m, PhH-4), 7.43-7.40 (2H, m, NPhH-2), 7.36-7.32 (3H, m, NPhH), 5.23 (1H, ABd, J 16.2, OCHAHB), 5.15 (1H, ABd, J 16.2, OCHAHB), 4.85 (1H, app dq, J 9.7, 5.9, BnCH), 4.01-3.93 (2H, m, OCH2CHBn), 3.50 (1H, ABX, JAB 13.6, JAX 5.9, PhCHAHB) and 3.18 (1H, ABX, JBA 13.6, JBX 9.7, PhCHAHB); δC (100 MHz, DMSO-d6) 149.9 (NCHN), 135.1 (NC), 134.9 (NArC-1), 134.9 (CH2PhC-1), 130.8 (ArCH-4), 130.4 (ArCH), 129.5 (ArCH), 129.0 (ArCH), 127.5 (ArCH), 120.7 (ArCH), 65.1 (OCH2), 61.5 (OCH2), 56.3 (NCH) and 37.5 (Ph-CH2); m/z MS (ESI+) 292 (100, [M-BF4]+); HRMS (ESI+) inlMMLBox ([M-BF4]+) requires 292.1444, found 292.1443 (-0.4 ppm); IR νmax (KBr)/cm-1 3337, 3141, 3060 (Ar C-H), 3026, 2987, 2969, 1585 (CN), 1536, 1497 (Ar CC), 1469, 1118 (C-O) and 1054 (br). |
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