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18162-48-6872-50-4Methylene ChloridenaphthaleneTHFTitanium Dioxide
ChemicalBook CAS DataBase List 1-(5H-Dibenzo[b,f]azepine-5-yl)ethanone
19209-60-0

1-(5H-Dibenzo[b,f]azepine-5-yl)ethanone synthesis

5synthesis methods
Iminostilbene

256-96-2
302 suppliers
$5.00/100mg

75-36-5 Synthesis
Acetyl chloride

75-36-5
591 suppliers
$17.92/100G

1-(5H-Dibenzo[b,f]azepine-5-yl)ethanone

19209-60-0
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Yield:19209-60-0 100%

Reaction Conditions:

Stage #1: dibenzoazepinewith sodium hydride in N,N-dimethyl-formamide;mineral oil;Inert atmosphere;
Stage #2: acetyl chloride in N,N-dimethyl-formamide;mineral oil at 23; for 1 h;Inert atmosphere;

Steps:

5-Acetyl-5H-dibenz[b,f]azepine (4); Typical Procedure

To a solution of iminostilbene (2; 965 mg, 5.0 mmol) in DMF (4 mL) at 0 °C under argon were added successively NaH (60% in oil; 240 mg,6.0 mmol) and AcCl (0.47 mL, 6.0 mmol), and the mixture was stirred at 23 °C for 1 h. The reaction was quenched with ice-water and the mixture was extracted with EtOAc. The organic layer was washed with sat. aq NaHCO3, dried over MgSO4, and concentrated in vacuo. The residue was purified by silica gel column chromatography (EtOAc-hexane, 1:2) to give 4 as a white solid; yield: 1.27 g (quant); mp 106 °C. IR (ATR): 1677 cm-1. 1H NMR (600 MHz, CDCl3): δ = 7.45-7.29 (m, 8 H), 6.96 (d, J = 12 Hz, 1H), 6.90 (d, J = 12 Hz, 1 H), 1.85 (s, 3 H). 13C NMR (150 MHz, CDCl3): δ = 170.8, 140.5, 140.3, 134.7, 133.5, 131.5, 129.3, 129.3, 129.3, 129.2, 129.0, 128.5, 127. 9, 127.9, 127.4, 22.1. HRMS (ESI): m/z [M + Na]+ calcd for C16H13NO: 258.0889; found: 258.0886.

References:

Kanase, Yuki;Kuniyoshi, Mai;Tabata, Hidetsugu;Takahashi, Yuka;Kayama, Susumu;Wakamatsu, Shintaro;Oshitari, Tetsuta;Natsugari, Hideaki;Takahashi, Hideyo [Synthesis,2015,vol. 47,# 24,art. no. SS-2015-F0451-OP,p. 3907 - 3913]

Iminostilbene

256-96-2
302 suppliers
$5.00/100mg

Acetic anhydride

108-24-7
0 suppliers
$14.00/250ML

1-(5H-Dibenzo[b,f]azepine-5-yl)ethanone

19209-60-0
14 suppliers
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References
5-ACETYLIMINODIBENZYL 99

13080-75-6
51 suppliers
$150.00/1g

1-(5H-Dibenzo[b,f]azepine-5-yl)ethanone

19209-60-0
14 suppliers
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References
Ethanone, 1-(10,11-dibromo-10,11-dihydro-5H-dibenz[b,f]azepin-5-yl)-

4614-45-3
0 suppliers
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7381-15-9 Synthesis
1,2-diphenyl-1,2-disodiumethane

7381-15-9
0 suppliers
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1-(5H-Dibenzo[b,f]azepine-5-yl)ethanone

19209-60-0
14 suppliers
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103-30-0 Synthesis
TRANS-STILBENE

103-30-0
200 suppliers
$9.00/5g

References
Ethanone, 1-(10-bromo-5H-dibenz[b,f]azepin-5-yl)-

28941-65-3
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1-(5H-Dibenzo[b,f]azepine-5-yl)ethanone

19209-60-0
14 suppliers
inquiry

References