4-[2-(2,4-DiMethylphenylsulfanyl)phenyl]piperazine-1-carboxylic acid tert-butyl ester synthesis
- Product Name:4-[2-(2,4-DiMethylphenylsulfanyl)phenyl]piperazine-1-carboxylic acid tert-butyl ester
- CAS Number:960203-42-3
- Molecular formula:C23H30N2O2S
- Molecular Weight:398.56
508233-74-7
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Yield:960203-42-3 95.1%
Reaction Conditions:
in dichloromethane at 25; for 1 h;
Steps:
2 Example 2: Preparation of 4-[2-(2,4-dimethylphenylsulfanyl)phenyl]Pyridazine-1-carboxylic acid tert-butyl ester (Formula-4)
Dissolve 1-[2-(2,4-dimethylphenylsulfanyl)phenyl]pyridazine (Formula 3,10.0g, 3.35mmol) in 20ml of methylene chloride followed by the addition of BOC anhydride (925yl). , 4.02 mmol), start stirring and react at 25 °C for 1 h.10 ml of water was added to the reaction flask, stirred for 0.5 h, and allowed to stand and separate. The aqueous layer was extracted twice with 10 ml of dichloromethane.The organic layers were combined and the solvent was evaporated under reduced pressure to give the product 1 · 27 g. Yield: 95.1 %. 1H NMR (400 MHz, CDCl3) δ 7.36 (d, J = 8.0Ηζ, 1Η), 7.15 (s, lH), 7.10-7.09 (m, 3H), 6.87 (t, J = 8.0Ηζ, 1Η), 6.53 ( d, J = 8.0Ηz, 1Η), 3.61 (t, J = 4.0Η1, 4Η), 3.01(s, 4H), 2.36 (s, 3Η), 2.32 (s, 3H), 1 · 52 (d, J = 16Hz, 9Η) See Fig. 2 13C NMR (101ΜΗz, CDCI3) δ 154.95, 149.01, 142.36, 139.25, 136.12, 134.65, 131.71, 127.87, 127.83, 126.34, 125.54, 124.62, 119.91, 79.68, 51.63, 28.49, 21.20, 20.61 See Figure 3.
References:
CN108047162,2018,A Location in patent:Paragraph 0050; 0051
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960203-41-2
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