Heptane → HCID 178470069, compound

HRID 1766095Notes

Reaction equation

[NH2:1][C:2]([C:14]1[C:15]([C:23]2[CH:28]=[CH:27][CH:26]=[C:25]([N+:29]([O-:31])=[O:30])[CH:24]=2)=[N:16][C:17]([S:21][CH3:22])=[N:18][C:19]=1[NH2:20])=[C:3]([C:9]([O:11][CH2:12][CH3:13])=[O:10])[C:4]([O:6]CC)=O.CCCCCCC>C1(OC2C=CC=CC=2)C=CC=CC=1>[NH2:1][C:2]1[C:14]2[C:15]([C:23]3[CH:28]=[CH:27][CH:26]=[C:25]([N+:29]([O-:31])=[O:30])[CH:24]=3)=[N:16][C:17]([S:21][CH3:22])=[N:18][C:19]=2[N:20]=[C:4]([OH:6])[C:3]=1[C:9]([O:11][CH2:12][CH3:13])=[O:10]

Participants

Conditions

Temperature: 240 °C

Procedure

A suspension of diethyl 2-(amino-[6-amino-2-methylthio-4-(3-nitrophenyl)-pyrimidin-5-yl]-methylene)-malonate (example 30b, 1.34 g) in diphenyl ether (30 ml) was heated under a stream of nitrogen to 240° C. for 2 h. After the mixture was cooled to room temperature, heptane was added (200 ml) and the solids were collected by filtration. The title compound was purified by chromatography on silica gel using CH2Cl2/acetone=1/0 to 4/1 (v/v) as eluent.

Workup

temperatureAfter the mixture was cooled to room temperature
filtrationthe solids were collected by filtration
customThe title compound was purified by chromatography on silica gel

Sources & evidence

ORD record: ord-8f7a7ff53ba440e19ccc282001d45dca
Source dataset: uspto-grants-2007_06
DOI: 10.6084/m9.figshare.5104873.v1
Patent number: US07229990B2

Reaction notes

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