Bromine → HCID 178515242, compound

HRID 222098Notes

Reaction equation

HRID 222098 reaction equation
[N:1]1[NH:2][CH:3]=[C:4]2[C:9]=1[CH2:8][CH2:7][CH2:6][C:5]2=[O:10].[Br:11]Br>CCOCC.CC(O)=O>[Br:11][CH:6]1[CH2:7][CH2:8][C:9]2[C:4](=[CH:3][NH:2][N:1]=2)[C:5]1=[O:10]

Participants

5

Reactant 2

HCID 24408BromineHCID 178515920HCID 178515920, compound

Product 1

HCID 178515242HCID 178515242, compoundYield 80%

Reagents, catalysts & solvents 2

HCID 176Acetic AcidSolvent2×HCID 3283Diethyl EtherSolvent

Procedure

To a solution of 2,5,6,7-tetrahydro-indazol-4-one (5.28 mmol), optionally protected as the trityl derivative, in Et2O (20 mL) and AcOH (15 mL), at 0° C., a solution of Br2 (10.56 mmol) in AcOH (20 mL) was slowly added dropwise. The solution was then heated at 60° C. for 1h then the organic solvents were evaporated to dryness and the white precipitate was suspended in Et2O, filtered and dried. The title compound was obtained in 80% yield. ESI (+) MS: m/z 216 (MH+).

Workup

  1. customthe organic solvents were evaporated to dryness
  2. filtrationfiltered
  3. customdried

Sources & evidence

ORD record
ord-4702a11fa56942a98aad806e69315a3a
Source dataset
uspto-grants-2012_06
Patent number
US08207180B2

Reaction notes

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