HuagongsheHuagongshe Chemistry Print Report · For research reference only
Methanol → HCID 131728493, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Methanol | HCID 887 | — |
| Reactant | Cyclohexylamine | HCID 7965 | — |
| Reactant | 2-[Bis-(2-chloroethyl)amino]-4-chloro-6-methyl-10,10-dioxo-10,11-dihydro-5-oxa-10lambda*6*-thia-dibenzo[a,d]-cycloheptene-8-carboxylic acid | HCID 131728474 | — |
| Product | HCID 131728493 | HCID 131728493 | — |
Reaction Steps
Cyclohexylamine (0.7 mL 6.25 mmol) was added to a solution of Example 102j (0.6 g, 1.25 mmol) in methanol (10 mL), followed by the addition of n-tetrabutylammonium iodide (0.010 g, 0.027 mmol) in an atmosphere of nitrogen and sealed in a pressure reactor vessel at 110° C. for 6 h. It was processed as described in the synthesis of Example 129k to obtain the title compound as a white solid. Yield: 0.290 g, (45.95%); 1H NMR (DMSO-d6): δ 1.10-2.00 (m, 1H, cyclohexyl), 2.70 (s, 3H, CH3), 3.20-3.30 (m, 4H, 2CH2), 3.75-3.8 (m, 4H, 2CH2), 3.95 (s, 3H, OCH3), 4.75 (s, 2H, CH2), 6.70 (s, 1H, Ar), 6.90 (s, 1H, Ar), 8.05 (s, 1H, Ar), 8.45 (s, 1H, Ar); MS: m/e (CI+) 519 (M+1).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07834001B2 |
| Source dataset | uspto-grants-2010_11 |
| ORD ID | ord-40d0fc7ad11042e586a67a8f61087a8e |
| Source note | uspto-grants-2010_11 |