Hydrochloric Acid → 1-[6-(2,6-Dichlorophenyl)-2-{[4-(diethylamino)butyl]amino}pyrido[2,3-d]pyrimidin-7-yl]-3-ethylurea

HRID 3440

Reaction equation

HRID 3440 reaction equation
[Cl:1][C:2]1[CH:7]=[CH:6][CH:5]=[C:4]([Cl:8])[C:3]=1[C:9]1[C:28]([NH:29][C:30]([NH:32][CH2:33][CH3:34])=[O:31])=[N:27][C:12]2[N:13]=[C:14]([NH:17][CH2:18][CH2:19][CH2:20][CH2:21][N:22]([CH2:25][CH3:26])[CH2:23][CH3:24])[N:15]=[CH:16][C:11]=2[CH:10]=1.Cl>O>[ClH:1].[Cl:1][C:2]1[CH:7]=[CH:6][CH:5]=[C:4]([Cl:8])[C:3]=1[C:9]1[C:28]([NH:29][C:30]([NH:32][CH2:33][CH3:34])=[O:31])=[N:27][C:12]2[N:13]=[C:14]([NH:17][CH2:18][CH2:19][CH2:20][CH2:21][N:22]([CH2:25][CH3:26])[CH2:23][CH3:24])[N:15]=[CH:16][C:11]=2[CH:10]=1.[Cl:1][C:2]1[CH:7]=[CH:6][CH:5]=[C:4]([Cl:8])[C:3]=1[C:9]1[C:28]([NH:29][C:30]([NH:32][CH2:33][CH3:34])=[O:31])=[N:27][C:12]2[N:13]=[C:14]([NH:17][CH2:18][CH2:19][CH2:20][CH2:21][N:22]([CH2:25][CH3:26])[CH2:23][CH3:24])[N:15]=[CH:16][C:11]=2[CH:10]=1

Participants

5

Procedure

To a solution of 1-[6-(2,6-dichlorophenyl)-2-(4-diethylamino-butylamino)-pyrido[2,3-d]pyrimidin-7-yl]-3-ethyl-urea (3.253 g) from Example 55 in water (250 mL) was added one equivalent of 1N hydrochloric acid (6.44 mL). The solution was stirred at room temperature until the solid was dissolved, filtered, and frozen. Lyophilization gave 3.63 g the hydrochloric acid salt of 1-[6-(2,6-dichlorophenyl)-2-(4-diethylamino-butylamino)-pyrido[2,3-d]pyrimidin-7-yl]-3-ethyl-urea, ESMS (20/80 MeOH/CH3CN+1% AcOH): M+ +H=504; mp dec >50° C.

Workup

  1. dissolutionwas dissolved
  2. filtrationfiltered
  3. temperaturefrozen

Sources & evidence

ORD record
ord-62852d9a12b3459797e4f780f0a64cab
Source dataset
uspto-grants-1998_03
Patent number
US05733913

Linked notes

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