HuagongsheHuagongshe Chemistry Print Report · For research reference only
Methanol → HCID 131728494, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Methanol | HCID 887 | — |
| Reactant | (2-Thienylmethyl)amine | HCID 34005 | — |
| 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 131728494 | HCID 131728494 | — |
Reaction Steps
Thiophenemethylamine (0.5 g 4.41 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: 0.370 g, (55.38%); 1H NMR (DMSO-d6): δ 2.55-2.60 (m, 4H, 2CH2), 2.70 (s, 3H, CH3), 3.20-3.55 (m, 4H, 2CH2), 3.75 (s, 3H, CH3), 3.95 (s, 3H, OCH3), 4.65 (s, 2H, CH2), 6.75 (s, 1H, Ar), 6.90 (s, 1H, Ar), 6.95-7.05 (m, 2H, Ar), 7.30 (s, 1H, Ar), 8.10 (s, 1H, Ar), 8.40 (s, 1H, Ar); MS: m/e (CI+) 533 (M+1).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07834001B2 |
| Source dataset | uspto-grants-2010_11 |
| ORD ID | ord-86985f3d19de4b04b6fdaec793d45308 |
| Source note | uspto-grants-2010_11 |