HCID 58365085, compound → HCID 67255739, compound

HRID 60253Notes

Reaction equation

C([O:3][C:4](=[O:26])[C:5]([NH:22]C(=O)C)([CH2:11][C:12]1[C:20]2[C:15](=[N:16][CH:17]=[CH:18][C:19]=2[Cl:21])[NH:14][CH:13]=1)C(OCC)=O)C>Cl>[ClH:21].[NH2:22][CH:5]([CH2:11][C:12]1[C:20]2[C:15](=[N:16][CH:17]=[CH:18][C:19]=2[Cl:21])[NH:14][CH:13]=1)[C:4]([OH:26])=[O:3]

Participants

Conditions

Temperature: 100 °C

Procedure

2-Acetylamino-2-(4-chloro-1H-pyrrolo[2,3-b]pyridin-3-ylmethyl)malonic acid diethyl ester (8.5 g, 22.3 mol) was dissolved in concentrated hydrochloric acid (45 mL) and the solution heated at 100° C. for 16 hours. The mixture was allowed to cool to ambient temperature and evaporated in-vacuo. The resultant residue was azeotroped with methanol (100 mL) and toluene (2×100 mL) to afford the crude title compound as a white solid. LCMS (Method B): RT=1.88 min, M+H+=240.

Workup

temperatureto cool to ambient temperature
customevaporated in-vacuo
customThe resultant residue was azeotroped with methanol (100 mL) and toluene (2×100 mL)

Sources & evidence

ORD record: ord-fd8d784a86d040baa05fe01011026821
Source dataset: uspto-grants-2016_09
DOI: 10.6084/m9.figshare.5104873.v1
Patent number: US09440976B2

Reaction notes

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