Fertile
Bluelighter
- Joined
- Mar 31, 2022
- Messages
- 1,627
Not hard to see why it's never turned up.
1,4-dimethoxybenzene -> 2,5-dimethoxybenzenesulfonyl chloride
2,5-dimethoxybenzenesulfonyl chloride -> 2,5-dimethoxythiophenol
2,5-dimethoxythiophenol -> 2,5-dimethoxyphenyl 2-methoxyethyl sulfide
2,5-dimethoxyphenyl 2-methoxyethyl sulfide -> 2,5-dimethoxy-4-(2-methoxyethylthio)benzaldehyde
2,5-dimethoxy-4-(2-methoxyethylthio)benzaldehyde -> 2,5-dimethoxy-4-(2-methoxyethylthio)-beta-nitrostyrene
2,5-dimethoxy-4-(2-methoxyethylthio)-beta-nitrostyrene -> 2,5-dimethoxy-4-(2-methoxyethylthio)phenethylamine
2,5-dimethoxy-4-(2-methoxyethylthio)phenethylamine -> 2-CT-13 NBOMe
165g of the first compound becomes about 5 grams of product & in the first step it looks like Shulgin was using 5l RB flask (given the volume of water, DCM, chlorosulfonic acid and the solid precursors). It's possible but it's quite a brisk writeup and so I wouldn't even expect to get CLOSE to that yield until each step had been optimised. Even Shulgin notes the huge amount of work involved, and he didn't even do the last, admittedly simple step.
One would keep stepping down scale at each step so that if you mess it up, you don't have to 'start at the top' again. It's, well, daunting.
1,4-dimethoxybenzene -> 2,5-dimethoxybenzenesulfonyl chloride
2,5-dimethoxybenzenesulfonyl chloride -> 2,5-dimethoxythiophenol
2,5-dimethoxythiophenol -> 2,5-dimethoxyphenyl 2-methoxyethyl sulfide
2,5-dimethoxyphenyl 2-methoxyethyl sulfide -> 2,5-dimethoxy-4-(2-methoxyethylthio)benzaldehyde
2,5-dimethoxy-4-(2-methoxyethylthio)benzaldehyde -> 2,5-dimethoxy-4-(2-methoxyethylthio)-beta-nitrostyrene
2,5-dimethoxy-4-(2-methoxyethylthio)-beta-nitrostyrene -> 2,5-dimethoxy-4-(2-methoxyethylthio)phenethylamine
2,5-dimethoxy-4-(2-methoxyethylthio)phenethylamine -> 2-CT-13 NBOMe
165g of the first compound becomes about 5 grams of product & in the first step it looks like Shulgin was using 5l RB flask (given the volume of water, DCM, chlorosulfonic acid and the solid precursors). It's possible but it's quite a brisk writeup and so I wouldn't even expect to get CLOSE to that yield until each step had been optimised. Even Shulgin notes the huge amount of work involved, and he didn't even do the last, admittedly simple step.
One would keep stepping down scale at each step so that if you mess it up, you don't have to 'start at the top' again. It's, well, daunting.