HCID 19710466, compound → HCID 19710471, compound
Reaction equation
[N+:1]([C:4]1[CH:9]=[CH:8][CH:7]=[CH:6][C:5]=1[NH:10][CH2:11][CH2:12][CH2:13][CH2:14][CH2:15][CH2:16][CH2:17][CH2:18][CH2:19][CH2:20][CH2:21][CH2:22][NH:23][C:24]1[CH:29]=[CH:28][CH:27]=[CH:26][C:25]=1[N+:30]([O-])=O)([O-])=O>Cl>[NH2:30][C:25]1[CH:26]=[CH:27][CH:28]=[CH:29][C:24]=1[NH:23][CH2:22][CH2:21][CH2:20][CH2:19][CH2:18][CH2:17][CH2:16][CH2:15][CH2:14][CH2:13][CH2:12][CH2:11][NH:10][C:5]1[CH:6]=[CH:7][CH:8]=[CH:9][C:4]=1[NH2:1]Participants
3
Reactant 1
Product 1
Reagents, catalysts & solvents 1
Conditions
- Temperature
- 100 °C
Procedure
20 g (0.045 mol) N,N'-bis(2-nitrophenyl)-1,12-diaminododecane are dissolved in 100 ml concentrated hydrochloric acid, and 43 g (0.19 mol) stannochloride dihydrate dissolved in 50 ml concentrated hydrochloric acid are added. The mixtured is heated to approxiately 100° C. while stirred, and after three hours the product separated off is cooled. The water phase is separated off, and the product is suspended in 200 ml hot water, whereafter it is poured into 500 ml 2M sodium hydroxide. The released tetraamine is extracted twice with 150 ml methylchloride, and the organic phase is dried over magnesium sulphate and evaporated, whereby the product is crystallized. Yield 17.30 g (100%), melting point 85° to 88° C.
Workup
- additionare added
- customafter three hours the product separated off
- temperatureis cooled
- customThe water phase is separated off
- additionis poured into 500 ml 2M sodium hydroxide
- extractionThe released tetraamine is extracted twice with 150 ml methylchloride
- dry with materialthe organic phase is dried over magnesium sulphate
- customevaporated
- customwhereby the product is crystallized
Sources & evidence
- ORD record
- ord-13a0dd832efa444384bcef3e2bc19d15
- Source dataset
- uspto-grants-1998_01
- Patent number
- US05708123
Reaction notes
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