HCID 12542767, compound → HCID 59216298, compound

HRID 2245962Notes

Reaction equation

HRID 2245962 reaction equation
[Br:1][C:2]1[CH:7]=[CH:6][C:5]([C:8]2[N:13]=[N:12][C:11]([NH:14][NH2:15])=[N:10][CH:9]=2)=[CH:4][CH:3]=1.[S:16]1[C:20]2[CH:21]=[C:22]([C:25]3([C:28](O)=O)[CH2:27][CH2:26]3)[CH:23]=[CH:24][C:19]=2[N:18]=[CH:17]1>P(Cl)(Cl)(Cl)=O>[S:16]1[C:20]2[CH:21]=[C:22]([C:25]3([C:28]4[N:12]5[N:13]=[C:8]([C:5]6[CH:4]=[CH:3][C:2]([Br:1])=[CH:7][CH:6]=6)[CH:9]=[N:10][C:11]5=[N:14][N:15]=4)[CH2:27][CH2:26]3)[CH:23]=[CH:24][C:19]=2[N:18]=[CH:17]1

Participants

4

Reactant 2

HCID 12542767HCID 12542767, compoundHCID 59216340HCID 59216340, compound

Product 1

HCID 59216298HCID 59216298, compound

Reagents, catalysts & solvents 1

HCID 24813Phosphorus oxychlorideSolvent

Conditions

Temperature
130 °C

Procedure

A mixture of 6-(4-bromophenyl)-3-hydrazino-1,2,4-triazine (20.0 mg, 0.0752 mmol) and 1-(1,3-benzothiazol-6-yl)cyclopropanecarboxylic acid (16.5 mg, 0.0752 mmol) in phosphoryl chloride (1 mL) was heated at 130° C. for 8 h. The volatiles were removed under reduced pressure. The residue was dissolved in methanol, and purified by RP-HPLC (pH=10) to give the desired product. LCMC: (M+H)+=448.9/451.0.

Workup

  1. customThe volatiles were removed under reduced pressure
  2. dissolutionThe residue was dissolved in methanol
  3. custompurified by RP-HPLC (pH=10)

Sources & evidence

ORD record
ord-f31b636b7c7d433dbb96ddabf125b988
Source dataset
uspto-grants-2010_03
Patent number
US07683060B2

Reaction notes

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