1-Chloro-4-Methylisoquinoline synthesis
- Product Name:1-Chloro-4-Methylisoquinoline
- CAS Number:24188-78-1
- Molecular formula:C10H8ClN
- Molecular Weight:177.63
77077-83-9
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24188-78-1
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Yield:24188-78-1 90%
Reaction Conditions:
Stage #1: 4-methyl-1(2H)-isoquinolinonewith trichlorophosphate for 3 h;Heating / reflux;
Stage #2: with sodium hydroxide in water;
Steps:
2.B.86.2
Step 2: A solution of 4-methyl-2H-isoquinolin-1-one (4.8 g) in POCl3 (50 mL) was refluxed for 3 hours. After cooling and concentration, the residue was based with 5 N NaOH and extracted with CH2Cl2. The organic layer was washed with brine and dried over MgSO4. After filtration and concentration, purification by flash chromatography of Biotage with 5% ethyl acetate in hexanes gave 4.8 g (90%) of the desired product as a solid. 1H NMR (400 MHz, CDCl3) 8 ppm 2.59 (s, 3H), 7.68 (t, J=7.70 Hz, 1H), 7.78 (m, 1H), 7.94 (d, J-8.31 Hz, 1H), 8.11 (s, 1H), 8.35 (d, J=8.31 Hz, 1H).
References:
US2006/183694,2006,A1 Location in patent:Page/Page column 73-74
103261-29-6
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24188-78-1
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$129.00/100mg
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24188-78-1
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24188-78-1
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$129.00/100mg