Methylamine → HCID 178482400, compound
Reaction equation
[N:1]1([C:10]2[N:18]=[C:17](Cl)[N:16]=[C:15]3[C:11]=2[N:12]=[CH:13][NH:14]3)[C:5]2[CH:6]=[CH:7][CH:8]=[CH:9][C:4]=2[N:3]=[CH:2]1.[CH3:20][NH2:21]>CS(C)=O>[N:1]1([C:10]2[N:18]=[C:17]([NH:21][CH3:20])[N:16]=[C:15]3[C:11]=2[N:12]=[CH:13][NH:14]3)[C:5]2[CH:6]=[CH:7][CH:8]=[CH:9][C:4]=2[N:3]=[CH:2]1Participants
4
Reactant 2
Product 1
Reagents, catalysts & solvents 1
Conditions
- Temperature
- 120 °C
Procedure
200 mg of product obtained in stage 1 above are mixed with 2 ml of DMSO and 0.115 ml (5 equivalents) of methylamine, and the mixture is then heated at 120° C. for approximately 18 hours. The mixture is allowed to return to ambient temperature. Purification is carried out by chromatography on silica with a CH2Cl2-MeOH—NH4OH: 90-9-1 mixture for eluent. Evaporation is carried out and a paste is formed in methylene chloride. Partial drying and drying under vacuum at 50° C. are carried out. 190 mg of expected product are obtained.
Workup
- customto return to ambient temperature
- customPurification
- customEvaporation
- customa paste is formed in methylene chloride
- customPartial drying
- customdrying under vacuum at 50° C.
Sources & evidence
- ORD record
- ord-31be6f77aead48008b67fdcdfb320223
- Source dataset
- uspto-grants-2009_01
- Patent number
- US07476670B2
Reaction notes
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