Hydrochloric Acid → HCID 70926616, compound

HRID 871877Notes

Reaction equation

HRID 871877 reaction equation
[NH2:1][C:2]1[N:32]([CH2:33][C:34]([OH:37])([CH3:36])[CH3:35])[C:6]2[N:7]=[C:8]([NH:11][C:12]3[CH:17]=[CH:16][C:15]([CH:18]4[CH2:23][CH2:22][N:21]([CH2:24][CH2:25][C:26]([F:29])([F:28])[F:27])[CH2:20][CH2:19]4)=[CH:14][C:13]=3[O:30][CH3:31])[N:9]=[CH:10][C:5]=2[C:4](=[O:38])[C:3]=1[C:39]([NH2:41])=[O:40].[ClH:42].CCOCC>CO.O1CCOCC1>[ClH:42].[NH2:1][C:2]1[N:32]([CH2:33][C:34]([OH:37])([CH3:36])[CH3:35])[C:6]2[N:7]=[C:8]([NH:11][C:12]3[CH:17]=[CH:16][C:15]([CH:18]4[CH2:23][CH2:22][N:21]([CH2:24][CH2:25][C:26]([F:27])([F:28])[F:29])[CH2:20][CH2:19]4)=[CH:14][C:13]=3[O:30][CH3:31])[N:9]=[CH:10][C:5]=2[C:4](=[O:38])[C:3]=1[C:39]([NH2:41])=[O:40]

Participants

6

Reactant 3

HCID 313Hydrochloric AcidHCID 3283Diethyl EtherHCID 67325452HCID 67325452, compound

Product 1

HCID 70926616HCID 70926616, compound

Reagents, catalysts & solvents 2

HCID 887MethanolSolventHCID 312751,4-DioxaneSolvent

Procedure

A solution of 0.70 g (1.22 mmol) of the product prepared in step 17.4 in 17 mL of methanol is cooled on an ice bath, and 0.91 mL (3.65 mmol) of a 4N solution of hydrogen chloride in dioxane is added. The mixture is stirred for 30 minutes at room temperature and is then poured into ether. The solid is drained by suction, rinsed with pentane and dried in an oven under vacuum. 0.64 g of the expected product is finally obtained in the form of a white solid. Yield (dihydrochloride)=91%. m.p.>260°C. M+H+=578

Workup

  1. washrinsed with pentane
  2. customdried in an oven under vacuum

Sources & evidence

ORD record
ord-55f8b5df919d4d5da458652a9cafb410
Source dataset
uspto-grants-2015_03
Patent number
US08975250B2

Reaction notes

Loading…