一二三四区视频,亚洲少妇熟女色,日本久热无码视频网,欧美国产日韩大尺度,亚洲a视频,久久少妇一区二区,日韩999无码视频,刺激久久久久久久,啊啊啊啊不要啊在线

Welcome to chemicalbook!
Chinese English Japanese Germany Korea
010-86108875
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 Bromonordiazepam
2894-61-3

Bromonordiazepam synthesis

10synthesis methods
-

Yield:612527-22-7 67%

Reaction Conditions:

with water;sodium carbonate in ethanol; for 5 h;Heating / reflux;

Steps:



suspension of 7-bromo-1,3-dihydro-5-phenyl-2H-1,4-benzodiazepin-2-thione 84 (1.6 g, 4.83 mmol), glycine (1.81 g, 24.2 mmol) and Na2CO3 (1.84 g, 17.4 mmol) in EtOH (38 mL)-H2O (16 mL) was stirred at reflux for 5 h, poured into water (100 mL), and then filtered to remove a small amount of 7-bromo-1,3-dihydro-5-phenyl-2H-1,4-benzodiazepin-2-one which remained. See Archer G A, Sternbach L H (1964) J Org Chem 29:231. The filtrate was extracted with CHCl3. The CHCl3 extract was discarded; the aqueous layer was adjusted to pH 4 with 2N HCl and then extracted with CHCl3 (3×25 mL). Evaporation of the CHCl3 solution gave pure acid 85 (1.2 g, 67%) as a yellow solid. Acid 85 (350 mg, 0.941 mmol) was suspended in dry CH2Cl2 (10 mL) and DCC (223 mg, 1.08 mmol) was added. The suspension which resulted was stirred at 40° C. for 2 h and then cooled to 0° C. It was filtered, and the solvent was removed under vacuum to give 8-bromo-2,4-dihydro-6-phenyl-1H-imidazo[1,2-a][1,4]benzodiazepin-1-one 86 as a brown oil. The cyclized product 86 (ca. 250 mg) was dissolved in dry benzene (6 mL), dimethylformamide diethylacetal (130 mg, 0.883 mmol) and triethylamine (89 mg, 0.883 mmol) were added. The solution which resulted was stirred at room temperature for 1 h and the solvent was removed under vacuum, The residue was then crystallized from EtOAc-MeOH to give 87 (200 mg, 70%). A solution of 87 (180 mg, 0.440 mmol) in dry toluene (5 mL) was treated with 1-methyl piperazine (1 mL) and heated to reflux for 5 h. The solvent was removed in vacuum to give a gum which crystallized from CH2Cl2-Et2O to furnish 88 (PS-I-35, 146 mg, 72%). mp>250° C.; IR (KBr) 3324, 2932, 2787, 1692, 1624, 1475, 1402, 1297, 1137, 933 cm-1; 1H NMR (CDCl3) δ 7.95 (d, 1H, J=8.8 Hz), 7.72 (dd, 1H, J=2.3 Hz, J=8.8 Hz), 7.58-7.55 (m, 2H), 7.49-7.37 (m, 4H), 7.17 (s, 1H), 5.01 (d, 1H, J=12 Hz), 4.50-4.60 (m, 1H), 4.20-4.30 (m, 1H), 4.16 (d, 1H, J=12 Hz), 3.50-3.58 (m, 2H), 2.40-2.60 (m, 4H), 2.34 (s, 3H); MS (m/z) 465 (100). Anal. Calcd. for C23H22N5OBr.H2O: C, 58.79; H, 4.95; N, 14.89. Found: C, 58.73; H, 4.86; N,

References:

US2006/3995,2006,A1 Location in patent:Page/Page column 48-49

南康市| 瑞安市| 商都县| 陆良县| 惠东县| 瑞丽市| 广宗县| 三门县| 平舆县| 溆浦县| 惠州市| 邵东县| 富阳市| 张家界市| 康马县| 安塞县| 五原县| 肥乡县| 阜城县| 红河县| 丹江口市| 辉县市| 沙雅县| 凤山县| 茶陵县| 成安县| 南澳县| 永康市| 疏勒县| 济源市| 榆中县| 泰宁县| 贡觉县| 苍南县| 达孜县| 读书| 香格里拉县| 荔浦县| 明光市| 临高县| 丰宁|