Hexane → HCID 57882275, compound

HRID 1817209Notes

Reaction equation

[C:1]([C:3](=[CH:9][NH:10][C:11]1[CH:12]=[CH:13][C:14]2[S:18](=[O:20])(=[O:19])[CH2:17][CH2:16][C:15]=2[CH:21]=1)[C:4]([O:6]CC)=O)#[N:2].CCCCCC>C1C=CC(C2C=CC=CC=2)=CC=1.C1C=CC(OC2C=CC=CC=2)=CC=1>[O:6]=[C:4]1[C:21]2[C:11](=[CH:12][CH:13]=[C:14]3[S:18](=[O:19])(=[O:20])[CH2:17][CH2:16][C:15]3=2)[NH:10][CH:9]=[C:3]1[C:1]#[N:2]

Participants

Conditions

Temperature: 290 °C

Procedure

1.5 g (0.85 mmol) of ethyl 2-cyano-3-[(1,1-dioxido-2,3-dihydro-1-benzothien-5-yl)amino]acrylate were suspended in 15 ml of Dowtherm A and heated in a metal bath at 290° C. for about 1 h. The reaction mixture was then cooled to RT. The mixture was subsequently mixed with hexane and stirred at RT for 30 min; the precipitate produced thereby was filtered off with suction and washed with hexane. 836 mg (65%) of the desired product were obtained in the form of brownish crystals.

Workup

temperatureThe reaction mixture was then cooled to RT
customthe precipitate produced
filtrationthereby was filtered off with suction
washwashed with hexane

Sources & evidence

ORD record: ord-ab7b17888d6443dea5f598682b77b859
Source dataset: uspto-grants-2009_10
DOI: 10.6084/m9.figshare.5104873.v1
Patent number: US07598263B2

Reaction notes

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