2-BROMO-4-(METHYLTHIO)PHENOL synthesis
- Product Name:2-BROMO-4-(METHYLTHIO)PHENOL
- CAS Number:131845-96-0
- Molecular formula:C7H7BrOS
- Molecular Weight:219.1
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Yield:131845-96-0 39%
Reaction Conditions:
with copper(I) oxide in N,N-dimethyl-formamide at 80; for 48 h;
Steps:
E
Method E: Preparation of 2-bromo-4-methylsulfanylphenol (XXI); [0080] Sodium thiomethoxide (8.64 g) and copper (I) oxide (8.79 g) were mixed with 2- bromo-4-iodophenol (XX, 14.72 g) in anhydrous DMF (100 mL). The mixture was stirred and heated at 80 0C for 48h under nitrogen atmosphere. Then, the resultant slurry was treated with concentrated HCl (5 mL) and EtOAc (200 mL), and was filtered and rinsed with EtOAc (200 mL). The organic layers were partitioned with IN HCl (150 mL), water (150 mL) and brine (150 mL) and dried over MgSO4, filtered and solvent removed in vacuo. Product was purified by silica gel column chromatography, the product eluted with dichloromethane/hexane (2:3), to give the desired product (5.22g, 39%) as a light brown oil.[0081] 1H NMR (400 MHz, CDCl3) δ 7.42 (IH, s), 7.19 (IH, d), 6.95 (IH, d), 5.40 (IH, s), 2.41 (3H, s).
References:
WO2008/39641,2008,A2 Location in patent:Page/Page column 19
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