Hydrochloric Acid → HCID 86700082, compound

HRID 1428138Notes

Reaction equation

HRID 1428138 reaction equation
[ClH:1].[NH2:2][C:3]1[C:8]([C:9]2[CH:14]=[CH:13][C:12]([NH:15][C:16]([C:18]3[C:23](=[O:24])[C:22]([C:25]4[CH:30]=[CH:29][C:28]([F:31])=[CH:27][CH:26]=4)=[CH:21][N:20]([CH2:32][C:33]([F:36])([F:35])[F:34])[CH:19]=3)=[O:17])=[CH:11][CH:10]=2)=[CH:7][C:6]([C:37]2[CH:42]=[CH:41][C:40]([O:43][CH3:44])=[C:39]([O:45][CH3:46])[CH:38]=2)=[CH:5][N:4]=1>CC(O)C>[OH2:17].[ClH:1].[NH2:2][C:3]1[C:8]([C:9]2[CH:10]=[CH:11][C:12]([NH:15][C:16]([C:18]3[C:23](=[O:24])[C:22]([C:25]4[CH:26]=[CH:27][C:28]([F:31])=[CH:29][CH:30]=4)=[CH:21][N:20]([CH2:32][C:33]([F:34])([F:35])[F:36])[CH:19]=3)=[O:17])=[CH:13][CH:14]=2)=[CH:7][C:6]([C:37]2[CH:42]=[CH:41][C:40]([O:43][CH3:44])=[C:39]([O:45][CH3:46])[CH:38]=2)=[CH:5][N:4]=1

Participants

4

Reactant 2

HCID 313Hydrochloric AcidHCID 71698834HCID 71698834, compound

Product 1

HCID 86700082HCID 86700082, compoundYield 92%

Reagents, catalysts & solvents 1

HCID 3776IsopropanolSolvent2×

Conditions

Temperature
40 °C

Procedure

2-Propanol (50 ml), concentrated hydrochloric acid (as 36%, d=1.18) (0.76 ml, 1.1 eq.) and 1.5% aqueous 2-propanol (50 ml) were added to the compound of Step 3 of Example 9 (5.00 g, 8.08 mmol) at room temperature. After warming to 40° C., the compound of Example 93 (10 mg) was seeded. The mixture was stirred at 40° C. for about two hours and then stirred at room temperature for 30 minutes, and the precipitated solid was collected by filtration. The solid was then dried under reduced pressure at 40° C. overnight to give the title compound (5.02 g). Yield: 92%.

Workup

  1. stirringstirred at room temperature for 30 minutes
  2. filtrationthe precipitated solid was collected by filtration
  3. customThe solid was then dried under reduced pressure at 40° C. overnight

Sources & evidence

ORD record
ord-dc30a37d3a6d49ffb2e04c8476146b41
Source dataset
uspto-grants-2015_01
Patent number
US08933103B2

Reaction notes

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