HuagongsheHuagongshe Chemistry Print Report · For research reference only
Dichloromethane methanol → HCID 66830431, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Dichloromethane methanol | HCID 21226129 | — |
| Reactant | HCID 66830431 | HCID 66830431 | — |
| Product | HCID 57853806 | HCID 57853806 | — |
| Product | 2-(2,5-Dichloropyrimidin-4-ylamino)-N-methylbenzamide | HCID 57974132 | — |
| Product | HCID 66830431 | HCID 66830431 | 30% |
Reaction Steps
2-[5-Chloro-2-(1-methyl-5-oxo-2,3,4,5-tetrahydro-1H-benzo[e][1,4]diazepin-7-ylamino)-pyrimidin-4-ylamino]-N-methylbenzamide. This compound was prepared according to the procedure for Example 417b. From 7-amino-1-methyl-1,2,3,4-tetrahydro-benzo[e][1,4]diazepin-5-one (75 mg, 0.39 mmol) and 2-(2,5-dichloro-pyrimidin-4-ylamino)-N-methylbenzamide (111 mg, 0.37 mmol) was obtained 48 mg (30%) of the title compound following preparative tlc (20% MeOH/DCM); m.p. 235-245° C. (dec.); MS: m/z/=452/454 (M+H)+, Cl-isotope pattern; 1H-NMR (DMSO-d6, δ): 11.64 (s, 1H), 9.36 (s, 1H), 8.75 (m, 2H), 8.19 (s, 2H), 7.76 (d, 7 Hz, 1H), 7.70 (m, 2H), 7.47 (t, 7 Hz, 1H), 7.11 (t, 7 Hz, 1H), 6.88 (d, 8 Hz, 1H), 3.13 (m, 4H), 2.79 (s, 3H), 2.75 (s, 3H).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08148391B2 |
| Source dataset | uspto-grants-2012_04 |
| ORD ID | ord-c1e94ad2fe2346a2a2b77f1ef5c2e352 |
| Source note | uspto-grants-2012_04 |