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ChemicalBook CAS DataBase List 2,3,4,5-TETRAHYDRO-1H-BENZO[B][1,4]DIAZEPINE

2,3,4,5-TETRAHYDRO-1H-BENZO[B][1,4]DIAZEPINE synthesis

4synthesis methods
-

Yield:6516-89-8 73.9%

Reaction Conditions:

with dimethylsulfide borane complex in tetrahydrofuran at 60; for 5 h;

Steps:

2.7 2.7 Preparation of Compound B20
2.7 Preparation of Compound B20 To a solution of compound 2 (3.3 g, 20 mmol) in THF (50 mL) was added BH3-Me2S (3 mL, 30 mmol). The mixture was heated to 60° C. for 5 h. The mixture was concentrated in vacuo. The residue was purified by silica gel chromatography (PE:EA=1:1) to give B20 as yellow solid (2.1 g, yield: 73.9%). 1H NMR (400 MHz, CDCl3): δ ppm: 6.85-6.71 (m, 4H), 3.09-2.97 (m, 4H), 1.95-1.86 (m, 2H). LCMS: 149 [M+1].

References:

Hartman, George D. US2015/132258, 2015, A1 Location in patent:Paragraph 0352; 0355; 0356

FullText

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