反应详情
EQUATION
反应方程式
REACTANTS
反应物
1,2-Cyclohexanediamine
C6H14N2
Thionyl chloride
Cl2OS
Cesium fluoride
CsF
4-bromobenzene-1,2-diamine
C6H7BrN2
未命名化合物
Hypochlorous acid, 1,1-dimethylethyl ester
C4H9ClO
未命名化合物
(3alpha)-6'-Methoxy-9-[(4-{[(4beta)-6'-methoxy-10,11-dihydrocinchonan-9-yl]oxy}phthalazin-1-yl)oxy]-10,11-dihydrocinchonan
C48H54N6O4
未命名化合物
Butyllithium
C4H9Li
PRODUCTS
产物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
The compound was synthesized according to method 5 starting from n-butyl lithium (2.3M in hexane; 3.66 mL, 7.32 mmol), tri phenyl phosphonium bromide (2.6 g, 7.32 mmol), 4-(4-morpholinocyclohexyl)benzaldehyde (1 g, 3.66 mmol), t-butyl hypochlorite (1.13 mL, 8.85 mmol), Boc carbamate (1.03 g, 8.85 mmol) 0.4M aqueous sodium hydroxide (360 mg in 10 mL), (DHQ)2PHAL (114 mg, mmol), potassium osmate dihydrate (40 mg, 0.12 mmol), thionyl chloride (0.6 mL, 8 mmol), 1,2-diamino-4-bromobenzene (160 mg, 0.84 mmol) and cesium fluoride (190 mg, 1.26 mmol), copper iodide (25 mg, 0.13 mmol) and 1,2-diaminocyclohexane (15 mg, 0.13 mmol), formic acid (10 mL). Yield: 40 mg (2.4%), MS m/z 447.4 (M+H)+; 1H-NMR (400 MHz, DMSO-d6): δ 12.38 (s, 1H); 8.15 (s, 1H); 7.60-7.16 (m, 6H); 5.69 (t, 1H); 4.8 (t, 1H); 4.13-4.10 (q, 1H); 3.57 (t, 4H); 2.56 (merged with DMSO, 1H); 2.33 (s, 4H); 2.11 (s, 1H); 1.91-1.67 (m, 5H); 1.45-1.38 (m, 4H), HPLC (λ=214 nm, [A]: rt 7.95 min (97.87%)
WORKUP
后处理
- customThe compound was synthesized
- customrt 7.95 min (97.87%)