Hydrochloric Acid → HCID 70926002, compound

HRID 871881Notes

Reaction equation

HRID 871881 reaction equation
[NH2:1][C:2]1[N:33]([CH2:34][C:35]([OH:38])([CH3:37])[CH3:36])[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](C(OC(C)(C)C)=O)[CH2:20][CH2:19]4)=[CH:14][C:13]=3[O:31][CH3:32])[N:9]=[CH:10][C:5]=2[C:4](=[O:39])[C:3]=1[C:40](=[O:42])[NH2:41].[ClH:43].CCOCC>ClCCl.O1CCOCC1>[ClH:43].[NH2:1][C:2]1[N:33]([CH2:34][C:35]([OH:38])([CH3:37])[CH3:36])[C:6]2[N:7]=[C:8]([NH:11][C:12]3[CH:17]=[CH:16][C:15]([CH:18]4[CH2:19][CH2:20][NH:21][CH2:22][CH2:23]4)=[CH:14][C:13]=3[O:31][CH3:32])[N:9]=[CH:10][C:5]=2[C:4](=[O:39])[C:3]=1[C:40]([NH2:41])=[O:42]

Participants

6

Reactant 3

HCID 313Hydrochloric AcidHCID 3283Diethyl EtherHCID 86673146HCID 86673146, compound

Product 1

HCID 70926002HCID 70926002, compound

Reagents, catalysts & solvents 2

HCID 6344DichloromethaneSolventHCID 312751,4-DioxaneSolvent

Procedure

A suspension of 2.28 g (3.92 mmol) of the product prepared in step 19.1 in 70 mL of dichloromethane is cooled on an ice-water bath, and 9.8 mL (39.20 mmol) of a 4N solution of hydrogen chloride in dioxane are added slowly. The mixture is stirred at room temperature for 1 hour, and ether is added. The solid is drained by suction, rinsed with pentane and dried in an oven. 2.2 g of the expected product are obtained in the form of a beige-coloured solid, which is used as obtained in the following step. Yield (dihydrochloride)=quantitative.

Workup

  1. temperatureis cooled on an ice-water bath
  2. washrinsed with pentane
  3. customdried in an oven

Sources & evidence

ORD record
ord-68b74895ef944809bc19e5ac8acad81b
Source dataset
uspto-grants-2015_03
Patent number
US08975250B2

Reaction notes

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