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ChemicalBook CAS DataBase List 6-Chloro-1-tetralone
26673-31-4

6-Chloro-1-tetralone synthesis

9synthesis methods
A solution of sodium nitrite (173 mg, 2.51 mmol) in water (5 mL) at 0 °C (ice-bath) was added to a magnetically stirred suspension of 6-Amino-1-tetralone (360 mg, 2.23 mmol) in aqueous hydrochloric acid (10 mL, 6 M) at 0 °C. This reaction mixture was added dropwise to a solution of copper(I) chloride (267 mg, 2.70 mmol) in concentrated hydrochloric acid (5 mL) at 0 °C. It was allowed to warm up to room 100 temperature and stirred for a further 2 h after which it was neutralised with solid sodium carbonate, extracted with ethyl acetate (3 × 20 mL) and concentrated in vacuo to give slightly yellow oil. This material was subjected to flash chromatography (50% chloroform in hexane) and concentration of the appropriate fractions afforded 6-chloro-1-tetralone  (180 mg, 45%) as a waxy solid.
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Yield:26673-31-4 88%

Reaction Conditions:

with tert.-butylnitrite;copper dichloride in acetonitrile at 60; for 0.75 h;

Steps:

13.a Step a4

CuCl2 (2.0 g, 15.0 mmol) and t-butyl nitrite (2.2 mL, 15.0 mmol) in dry CH3CN were heated at 60° C., followed by the addition of 6-aminotetralone (2.0 g, 12.0 mmol). The reaction mixture was heated for 45 min, then cooled down at room temperature, quenched with 2N HCl (200 mL) and Et2O (200 mL). The aqueous layer was extracted with Et2O and the combined organic layer was washed with water, brine, dried over anhydrous Na2SO4, concentrated by rotary evaporation, and purified by column chromatography to give 6-chloro-3,4-dihydronaphthalen-1(2H)-one (16) (88%). 111 NMR (600 MHz, CDCl3) δ 7.96 (d, J=6.0 Hz, 1H), 7.28-7.26 (m, 2H), 2.94 (t, J=6.0 Hz, 2H), 2.65 (t, J=6.0 Hz, 2H), 2.16-2.11 (m, 2H), 7.12-7.07 (m, 2H), 6.92 (d, J=12.0 Hz, 1H), 6.85 (s, 1H), 5.67 (s, 1H). GC-MS (ES) for C10H9C10 [M]+ 180.

References:

US2015/105351,2015,A1 Location in patent:Paragraph 0440

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