Hydrochloric Acid → HCID 60164763, compound

HRID 513774Notes

Reaction equation

[Li+].[OH-].C[O:4][C:5]([C:7]1[CH:24]=[C:23]2[C:10]([S:11](=[O:26])(=[O:25])[NH:12][C:13]3[C:22]2=[CH:21][CH:20]=[C:19]2[C:14]=3[N:15]=[CH:16][CH:17]=[CH:18]2)=[CH:9][CH:8]=1)=[O:6].Cl>CO>[O:26]=[S:11]1(=[O:25])[C:10]2[C:23](=[CH:24][C:7]([C:5]([OH:6])=[O:4])=[CH:8][CH:9]=2)[C:22]2[C:13](=[C:14]3[C:19](=[CH:20][CH:21]=2)[CH:18]=[CH:17][CH:16]=[N:15]3)[NH:12]1

Participants

Conditions

Temperature: 65 °C

Procedure

LiOH (9 mg, 0.21 mmol) was added to a solution of 6,6-dioxo-5,6-dihydro-6λ*6*-thia-4,5-diaza-chrysene-9-carboxylic acid methyl ester 307 (33 mg, 0.097 mmol) in MeOH (2 ml) and the mixture was heated at 65° C. for 18 h. After cooling, the pH was adjusted to 7-8 with methanolic HCl. The mixture was concentrated in vacuo. The crude residue was purified by column chromatography with DCM/MeOH (90:10) as the eluent to give the title compound (28 mg, 90%).

Workup

temperatureAfter cooling
concentrationThe mixture was concentrated in vacuo
customThe crude residue was purified by column chromatography with DCM/MeOH (90:10) as the eluent

Sources & evidence

ORD record: ord-47e128538776424bb104a87329d3664f
Source dataset: uspto-grants-2015_08
DOI: 10.6084/m9.figshare.5104873.v1
Patent number: US09102688B2

Reaction notes

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