成人免费xx,国产又黄又湿又刺激不卡网站,成人性视频app菠萝网站,色天天天天

Welcome to chemicalbook!
Chinese English Japanese Germany Korea
400-158-6606
Try our best to find the right business for you.
Do not miss inquiry messages Please log in to view all inquiry messages.

Welcome back!

ChemicalBook CAS DataBase List 7-chloro 5-(2-chlorophenyl)-1,3-dihydro-2H-(1,4)-benzodiazepine-2-thione
2894-71-5

7-chloro 5-(2-chlorophenyl)-1,3-dihydro-2H-(1,4)-benzodiazepine-2-thione synthesis

5synthesis methods
-

Yield:2894-71-5 81%

Reaction Conditions:

with Lawessons reagent in 1,2-dimethoxyethane at 80; for 5 h;

Steps:

4.1.4 Benzodiazepine-2-thiones 6a-d

A solution of 5a (114.8mg, 0.38mmol) in dimethoxyethane (1.9mL, 0.2M) containing Lawesson’s reagent (233.2mg, 0.58mmol) was stirred at 80°C for 5h. After the reaction was completed, the reaction mixture was cooled to rt and quenched with aq. NaHCO3. The reaction mixture was extracted with EtOAc (250mL), and the organic extract was washed with brine, dried (Na2SO4), and concentrated under reduced pressure. The residue was purified by column chromatography (hexane/EtOAc 2:1); yield: 98.6mg (81%); light yellow solid; mp 244-246°C (mp 252-253°C13, mp 240-241°C14b); Rf=0.40 (hexane/EtOAc 3:1). IR (ATR): 2959, 1474, 1179cm-1. 1H NMR (400MHz, CDCl3): δ 9.85 (br s, 1H), 7.54-7.52 (m, 1H), 7.46-7.36 (m, 4H), 7.11 (d, J=8.8Hz, 1H), 7.06 (d, J=2.4Hz, 1H), 4.81 (br s, 2H). 13C NMR (100MHz, CDCl3): δ 200.2, 168.9, 137.8, 137.2, 133.1, 131.9, 131.2, 131.2, 130.7, 130.5, 130.2, 129.6, 127.1, 122.2, 63.1. HRMS (ESI-TOF): m/z [M+H]+ calcd for C15H11N2SCl2: 321.0015; found: 321.0016.

References:

Tanaka, Ryoko;Makino, Kosho;Tabata, Hidetsugu;Oshitari, Tetsuta;Natsugari, Hideaki;Takahashi, Hideyo [Bioorganic and Medicinal Chemistry,2022,vol. 64,art. no. 116758]