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Type | HazMat fee for 500 gram (Estimated) |
Excepted Quantity | USD 0.00 |
Limited Quantity | USD 15-60 |
Inaccessible (Haz class 6.1), Domestic | USD 80+ |
Inaccessible (Haz class 6.1), International | USD 150+ |
Accessible (Haz class 3, 4, 5 or 8), Domestic | USD 100+ |
Accessible (Haz class 3, 4, 5 or 8), International | USD 200+ |
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CAS No. : | 1072901-09-7 | MDL No. : | MFCD28556923 |
Formula : | C16H21N3 | Boiling Point : | - |
Linear Structure Formula : | - | InChI Key : | - |
M.W : | 255.36 | Pubchem ID : | - |
Synonyms : |
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Signal Word: | Danger | Class: | 9 |
Precautionary Statements: | P501-P273-P260-P270-P264-P280-P391-P314-P337+P313-P305+P351+P338-P301+P312+P330 | UN#: | 3077 |
Hazard Statements: | H302-H319-H372-H410 | Packing Group: | Ⅲ |
GHS Pictogram: |
* All experimental methods are cited from the reference, please refer to the original source for details. We do not guarantee the accuracy of the content in the reference.
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
66% | With 1,1'-bis-(diphenylphosphino)ferrocene; tris-(dibenzylideneacetone)dipalladium(0); sodium t-butanolate; In toluene; at 100℃; for 72h;Glovebox; | Inside a glovebox, a 250?mL reaction vessel was charged with Pd2(dba)3 (1.36?g, 1.49?mmol), bis(diphenylphosphino)-ferrocene (DPPF) (1.65?g, 2.97?mmol), NaOt-Bu (9.84?g, 0.098?mol) and toluene (100?mL). 2-Bromo-N,N-dimethylaniline (14.6?g, 0.073?mol) and 2-amino-N,N-dimethylaniline 40 (9.95?g, 0.073?mol) were degassed and added to the reaction mixture. The brown solution was then stirred for 3 days at 100?C. The solution was then cooled to room temperature and filtered through Celite. Removal of the solvent yielded a dark liquid that was taken in dichloromethane (20?mL) and filtered through a silica plug. Removal of the solvent gave SI-1 as a brown solid (12.0?g, 0.048?mol, 66%) that was used without further purification. Spectral data was consistent with that reported in the literature. 48 |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
Multi-step reaction with 2 steps 1: not given 2: benzene-d6 |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
74% | In a flame dried flask, under Ar, HMeNN2 (SI-1) (0.50 g, 2.0 mmol) was dissolved in THF (6 mL) and the solution cooled to -78 C n-BuLi (0.80 mL, 2.1 mmol, 2.5 M in hexanes) was added to the solution dropwise. The solution was allowed to warm naturally and stir for 1 h at room temperature. The resultant solution was then transferred to a THF (6 mL) suspension of NiCl2(dme) (0.44 g, 2.0 mmol) at -78 C. The reaction was allowed to warm naturally and was left stirring overnight at room temperature. 26 The solvent was then removed and the dark brown oil was taken in benzene and filtered through celite. The brown oil was purified by recrystallization (layer diffusion of pentane in benzene at room temperature) to give (NNN)-NiCl (17) as a brown solid (0.52 g, 1.5 mmol, 74%). Spectral data was consistent with that reported in the literature. 32 |