HuagongsheHuagongshe Chemistry Print Report · For research reference only
tert-Butyl isocyanate → HCID 118061913, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | tert-Butyl isocyanate | HCID 62412 | — |
| Reactant | HCID 118062249 | HCID 118062249 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 118061913 | HCID 118061913 | 70.1% |
Reaction Steps
To a stirred solution of Intermediate 104F (2.4 g, 7.47 mmol) in THF (20 mL) was added 2-isocyanato-2-methylpropane (0.741 g, 7.47 mmol) and the reaction mixture was stirred for 1.5 h. The volatiles were evaporated under reduced pressure. The crude was purified by silica gel chromatography (120 g REDISEP® column, eluting with 28% EtOAc in hexane). Fractions containing the product were combined and evaporated to afford Intermediate 104G (2.2 g, 70%). MS(ES): m/z=421 [M+H]+; 1H NMR (400 MHz, DMSO-d6) δ ppm 6.25 (s, 1H), 4.72 (s, 2H), 4.25 (q, J=6.8 Hz, 2H), 4.10 (t, J=5.24 Hz, 2H), 3.75 (m, 2H), 1.30 (t, J=7.2 Hz, 3H) 1.28 (s, 9H).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09273058B2 |
| Source dataset | uspto-grants-2016_03 |
| ORD ID | ord-639e2c6b77be48d3a75d8d0e2c21f48e |
| Source note | uspto-grants-2016_03 |