Ether hydrochloride → HCID 69433061, compound

HRID 1269788Notes

Reaction equation

HRID 1269788 reaction equation
[NH:1]1[C:9]2[C:4](=[C:5]([O:10][C@H:11]3[CH2:16][CH2:15][CH2:14][C@H:13]([NH2:17])[CH2:12]3)[CH:6]=[CH:7][CH:8]=2)[CH:3]=[N:2]1.[ClH:18].C(OCC)C>C(O)C>[ClH:18].[NH:1]1[C:9]2[C:4](=[C:5]([O:10][C@H:11]3[CH2:16][CH2:15][CH2:14][C@H:13]([NH2:17])[CH2:12]3)[CH:6]=[CH:7][CH:8]=2)[CH:3]=[N:2]1

Participants

4

Reactant 2

HCID 10953452Ether hydrochlorideHCID 69431435HCID 69431435, compound

Product 1

HCID 69433061HCID 69433061, compoundYield 88%

Reagents, catalysts & solvents 1

HCID 702EthanolSolvent

Procedure

To a solution of the trans-3-(1H-indazol-4-yloxy)-cyclohexanamine (163.1 mg, 0.705 mmol) obtained in Example 326 in ethanol (3 ml) was added 1M-hydrochloric acid/diethyl ether (0.776 ml, 0.776 mmol) at room temperature. After 1 hour, the resulting solution was concentrated under reduced pressure, and the resulting oil was crystallized by the addition of acetonitrile, followed by filtration. The precipitate was dried under reduced pressure to obtain trans-3-(1H-indazol-4-yloxy)-cyclohexanamine hydrochloride (166 mg, 88%).

Workup

  1. concentrationthe resulting solution was concentrated under reduced pressure
  2. customthe resulting oil was crystallized by the addition of acetonitrile
  3. filtrationfollowed by filtration
  4. customThe precipitate was dried under reduced pressure

Sources & evidence

ORD record
ord-9f21bafb87234b379433342d3ebd1e96
Source dataset
uspto-grants-2007_04
Patent number
US07199147B2

Reaction notes

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