5H-Benzocycloheptene, 2-bromo-6,7,8,9-tetrahydro- synthesis
- Product Name:5H-Benzocycloheptene, 2-bromo-6,7,8,9-tetrahydro-
- CAS Number:51490-23-4
- Molecular formula:C11H13Br
- Molecular Weight:225.12
Yield: 67%
Reaction Conditions:
in chloroform at 0 - 45; for 0.75 h;Molecular sieve;
Steps:
136.1 Step 1
Compound (M-21) (2.00 g, 12.5 mmol) was dissolved in chloroform (25.0 mL), 4Å molecular sieve (400 mg,powder) was added, compound (M-22) (3.10 g, 18.8 mmol) was added at 0°C, and the mixture was stirred at 0°C for 5min. After stirring at 45°C for 40 min, the mixture was allowed to cool to room temperature. The solvent was evaporatedunder reduced pressure, and the residue was purified by silica gel column chromatography (n-hexane:ethyl acetate) togive compound (M-23) (yield 1.90 g, 67%)
References:
Kaken Pharmaceutical Co., Ltd.;WATANABE, Atsushi;SATO, Yuuki;OGURA, Keiji;TATSUMI, Yoshiyuki EP3351533, 2018, A1 Location in patent:Paragraph 0370; 0371
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