Technology Process of Stannane, (3-chloro-3-methyl-1-butynyl)triphenyl-
There total 1 articles about Stannane, (3-chloro-3-methyl-1-butynyl)triphenyl- which
guide to synthetic route it.
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synthetic route:
- Guidance literature:
-
With
n-butyllithium;
In
tetrahydrofuran;
BuLi in hexane was cautiously added under N2 at -100°C to a stirred soln. of propargylic chloride in THF, after 10 min Ph3SnCl was added, mixt. was stirred at -60°C for 0.5 h, allowed to warm to room temp.; mixt. was poured into satd. aq. NH4Cl, extd. with 1:1 ether-pentane, combined exts. were washed with water, dried over MgSO4, evapd. in vacuo;
DOI:10.1016/0022-328X(84)80703-2
- Guidance literature:
-
tetrakis(triphenylphosphine) palladium(0);
In
tetrahydrofuran;
a soln. of Pd(PPh3)4 (4 mol%) in THF was added under N2 to a stirred soln. of Me3SiCCZnCl in THF at -20°C followed by Ph3SnCCCMe2Cl, mixt. was stirred for 2 h at 40°C; purity of the product >=95%; mixt. was poured into satd. aq. NH4Cl, extd. with pentane, combined exts. were washed with water, dried over MgSO4, solvent was evapd. in vacuo, residue crystd. from methanol or purified by column chromy. (Al2O3, hexane);
DOI:10.1016/0022-328X(84)80703-2
- Guidance literature:
-
tetrakis(triphenylphosphine) palladium(0);
In
tetrahydrofuran;
a soln. of Pd(PPh3)4 (4 mol%) in THF was added under N2 to a stirred soln. of t-BuCH=C=CHZnCl in THF at -20°C followed by Ph3SnCCCMe2Cl, mixt. was stirred for 2 h at 40°C; purity of the product >=95%; mixt. was poured into satd. aq. NH4Cl, extd. with pentane, combined exts. were washed with water, dried over MgSO4, solvent was evapd. in vacuo, residue crystd. from methanol or purified by column chromy. (Al2O3, hexane);
DOI:10.1016/0022-328X(84)80703-2
