Hydrochloric Acid → HCID 86700082, compound

HRID 1428139Notes

Reaction equation

C(#N)C.[ClH:4].[NH2:5][C:6]1[C:11]([C:12]2[CH:17]=[CH:16][C:15]([NH:18][C:19]([C:21]3[C:26](=[O:27])[C:25]([C:28]4[CH:33]=[CH:32][C:31]([F:34])=[CH:30][CH:29]=4)=[CH:24][N:23]([CH2:35][C:36]([F:39])([F:38])[F:37])[CH:22]=3)=[O:20])=[CH:14][CH:13]=2)=[CH:10][C:9]([C:40]2[CH:45]=[CH:44][C:43]([O:46][CH3:47])=[C:42]([O:48][CH3:49])[CH:41]=2)=[CH:8][N:7]=1>O>[OH2:20].[ClH:4].[NH2:5][C:6]1[C:11]([C:12]2[CH:13]=[CH:14][C:15]([NH:18][C:19]([C:21]3[C:26](=[O:27])[C:25]([C:28]4[CH:29]=[CH:30][C:31]([F:34])=[CH:32][CH:33]=4)=[CH:24][N:23]([CH2:35][C:36]([F:37])([F:38])[F:39])[CH:22]=3)=[O:20])=[CH:16][CH:17]=2)=[CH:10][C:9]([C:40]2[CH:45]=[CH:44][C:43]([O:46][CH3:47])=[C:42]([O:48][CH3:49])[CH:41]=2)=[CH:8][N:7]=1

Participants

Conditions

Temperature: 40 °C

Procedure

Acetonitrile (39 ml), 6 N hydrochloric acid (565 μl, 1.05 eq.) and water (420 μl) were added to the compound of Step 3 of Example 9 (2.00 g, 3.23 mmol) at room temperature. The mixture was stirred at 40° C. for about seven hours, followed by the addition of water (8.75 ml). After confirming dissolution, the solution was stirred at 0° C. for about 10 hours and then allowed to stand at room temperature for about three days, and the precipitated solid was collected by filtration. The solid was then dried at room temperature to give the title compound (0.54 g). Yield: 24%.

Workup

dissolutiondissolution
stirringthe solution was stirred at 0° C. for about 10 hours
waitto stand at room temperature for about three days
filtrationthe precipitated solid was collected by filtration
customThe solid was then dried at room temperature

Sources & evidence

ORD record: ord-62de00942f4f470e884faadadbcff8a7
Source dataset: uspto-grants-2015_01
DOI: 10.6084/m9.figshare.5104873.v1
Patent number: US08933103B2

Reaction notes

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