Hydrochloric Acid → HCID 68523591, compound

HRID 1992370Notes

Reaction equation

HRID 1992370 reaction equation
OC(C(F)(F)F)=O.[NH2:8][CH2:9][CH2:10][CH2:11][N:12]1[CH2:19][CH:18]2[O:20][CH:14]([CH2:15][N:16]([CH2:21][CH2:22][O:23][C:24]3[CH:31]=[CH:30][C:27]([C:28]#[N:29])=[CH:26][C:25]=3[F:32])[CH2:17]2)[CH2:13]1.[ClH:33]>O1CCOCC1>[ClH:33].[NH2:8][CH2:9][CH2:10][CH2:11][N:12]1[CH2:19][CH:18]2[O:20][CH:14]([CH2:15][N:16]([CH2:21][CH2:22][O:23][C:24]3[CH:31]=[CH:30][C:27]([C:28]#[N:29])=[CH:26][C:25]=3[F:32])[CH2:17]2)[CH2:13]1

Participants

4

Reactant 2

HCID 313Hydrochloric AcidHCID 131727851HCID 131727851, compound

Product 1

HCID 68523591HCID 68523591, compound

Reagents, catalysts & solvents 1

HCID 312751,4-DioxaneSolvent2×

Procedure

4-{2-[7-(3-Amino-propyl)-9-oxa-3,7-diaza-bicyclo[3.3.1]non-3-yl]-ethoxy}-3-fluoro-benzonitrile TFA-salt (7.79 g, 11.3 mmol, from step (iii) above) was dissolved in dioxane (15 ml). HCl (14 ml of a 4M solution in dioxane was added. The HCl-salt precipitated, the dioxane was decanted off and to the solid was added dioxane (10 ml ) followed by HCl (4 ml in dioxane). The solvent was decanted off and the solid was dried under vacuum. The solid was dissolved in water (5 ml) and freeze dried giving 2.98 g of the title compound

Workup

  1. customThe HCl-salt precipitated
  2. customthe dioxane was decanted off and to the solid
  3. additionwas added dioxane (10 ml )
  4. customThe solvent was decanted off
  5. customthe solid was dried under vacuum
  6. dissolutionThe solid was dissolved in water (5 ml)
  7. customfreeze dried

Sources & evidence

ORD record
ord-edac341f90d64a5e988d5895ef0c0eee
Source dataset
uspto-grants-2010_01
Patent number
US07648985B2

Reaction notes

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