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HuagongsheHuagongshe Chemistry Print Report · For research reference only
HRID 1040893Generated: October 30, 2026

Dichloromethane methanol → HCID 66830431, compound

https://huagongshe.com/reaction/1040893

Reaction equation

Participants

RoleNameHCIDCharge
ReactantDichloromethane methanolHCID 21226129—
ReactantHCID 66830431HCID 66830431—
ProductHCID 57853806HCID 57853806—
Product2-(2,5-Dichloropyrimidin-4-ylamino)-N-methylbenzamideHCID 57974132—
ProductHCID 66830431HCID 6683043130%

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

DOI10.6084/m9.figshare.5104873.v1
Patent numberUS08552186B2
Source datasetuspto-grants-2013_10
ORD IDord-fe8c57772b174bc89ccfcd78c4c759c3
Source noteuspto-grants-2013_10