HuagongsheHuagongshe Chemistry Print Report · For research reference only
Ethanolamine → HC Yellow no. 12
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Ethanolamine | HCID 700 | — |
| Reactant | 2,5-Dichloronitrobenzene | HCID 6977 | — |
| Solvent | 1-Butanol | HCID 263 | — |
| Product | HC Yellow no. 12 | HCID 5182864 | 86% |
Reaction Steps
A mixture of 1,4-dichloro-2-nitrobenzene (I-1, Aldrich, Wis.; 38.4 g, 0.2 mol) and 2-aminoethanol (24.4 g, 0.4 mol, 2 eq.) in n-butanol (100 mL) was refluxed overnight. The solvent was evaporated and the residue was dispersed in petrol ether (600 mL) and stirred overnight. The solids were filtered to give intermediate I-2 as a yellow powder (37 g, 86%). 1H-NMR (400 MHz, CDCl3): δ 8.24 (s, 1H), 8.19˜8.20 (d, 1H, J=2.4 Hz), 7.39˜7.42 (dd, 1H, J1=2.4 Hz, J2=9.2 Hz), 6.87˜6.90 (d, 1H, J=9.6 Hz), 3.95˜3.98 (t, 2H, J=5.2 Hz), 3.49˜3.53 (dd, 2H, J1=4.8 Hz, J2=10.4 Hz). MS (ESI): m/z 217 (M+H+).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08063032B2 |
| Source dataset | uspto-grants-2011_11 |
| ORD ID | ord-fda71cc00bfa40cc88e2a1bf3413119e |
| Source note | uspto-grants-2011_11 |