Diethyl Ether → HCID 70926404, compound

HRID 871873Notes

Reaction equation

HRID 871873 reaction equation
[CH2:1]([N:3]1[C:8]2[N:9]=[C:10]([NH:13][C:14]3[CH:19]=[CH:18][C:17]([CH:20]4[CH2:25][CH2:24][N:23]([CH2:26][CH2:27][C:28]([F:31])([F:30])[F:29])[CH2:22][CH2:21]4)=[CH:16][C:15]=3[O:32][CH3:33])[N:11]=[CH:12][C:7]=2[C:6](=[O:34])[C:5]([C:35]([NH2:37])=[O:36])=[C:4]1[NH:38][CH3:39])[CH3:2].CC[Cl:42].CCOCC>ClCCl.CO>[ClH:42].[CH2:1]([N:3]1[C:8]2[N:9]=[C:10]([NH:13][C:14]3[CH:19]=[CH:18][C:17]([CH:20]4[CH2:21][CH2:22][N:23]([CH2:26][CH2:27][C:28]([F:31])([F:30])[F:29])[CH2:24][CH2:25]4)=[CH:16][C:15]=3[O:32][CH3:33])[N:11]=[CH:12][C:7]=2[C:6](=[O:34])[C:5]([C:35]([NH2:37])=[O:36])=[C:4]1[NH:38][CH3:39])[CH3:2]

Participants

5

Reactant 3

HCID 3283Diethyl EtherHCID 6337ChloroethaneHCID 67324890HCID 67324890, compound

Product 1

HCID 70926404HCID 70926404, compound

Reagents, catalysts & solvents 1

HCID 21226129Dichloromethane methanolSolvent

Procedure

To a solution of 0.08 g (0.15 mmol) of the product prepared in step 16.5 in 6 mL of a dichloromethane/methanol mixture (v/v=1/1) is added 0.44 mL (0.44 mmol) of a 1M solution of hydrochloric ether. The mixture is stirred for 1 hour at room temperature, and ether is then added. The solid is drained by suction, rinsed with pentane and dried in an oven under vacuum. 0.09 g of the expected product is finally obtained in the form of a yellow solid. Yield (dihydrochloride)=99%. M+H+=548.

Workup

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

Sources & evidence

ORD record
ord-1d3cdc8d8f79485ea03dd1f3f74cef3e
Source dataset
uspto-grants-2015_03
Patent number
US08975250B2

Reaction notes

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