Category: 116861-31-5

Application of 116861-31-5, A common heterocyclic compound, 116861-31-5, name is tert-Butyl (3-chloropropyl)carbamate, molecular formula is C8H16ClNO2, its traditional synthetic route has been very mature, but the traditional synthetic route has various shortcomings, such as complicated route, low yield, poor purity, etc, below Introduce a new synthetic route.

A mixture of l-(lR-pyrrolo[2,3-c]pyridin-2No.yl)ethanone oxime (Example 72) (100 mg, 0.42 mmol) and sodium hydride (18 mg of a 60% in mineral oil, 0.45 mmol) in N,N- dimethyl formamide (4 mL) was stirred for 0.5 h. N-Boc chloropropylamine (86 mg, 0.44 mmol) was added dropwise and the reaction mixture was heated at 60C for 3 h. After stirring at room temperature for 12 h, the reaction mixture was quenched with water (10 mL) and extracted with ethyl acetate (3 15 mL). The combined organic extracts were washed with water and brine, dried over sodium sulfate, and concentrated to an oil. Purification by Biotage chromatography (30 to 100% ethyl acetate in hexanes) produced tert-butyl 3- [[[phenyl(1H-pyrrolo[2,3-c]pyridin-2- yl) methylene]amino]oxy]propylcarbamate (76 mg, 46%) as a white solid: mp 52-58C; ESI MS m/z 395 [C22H26N403 + H]+; HPLC (Method A) 98.6% (AUC) , tR = 19.2 min.

The synthetic route of 116861-31-5 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; TAKEDA PHARMACEUTICAL COMPANY LIMITED; WO2005/97129; (2005); A2;,
Amide – Wikipedia,
Amide – an overview | ScienceDirect Topics

Researchers who often do experiments know that organic synthesis is a process of preparing more complex target molecules from simple raw materials through one or more chemical reactions. Generally, it requires fewer steps, and cheap raw materials. 116861-31-5, name is tert-Butyl (3-chloropropyl)carbamate, A new synthetic method of this compound is introduced below., category: amides-buliding-blocks

3,3′,3″-(benzene-1,3,5-triyltris(oxy))tris(propan-1-amine) (2-1b) NaH (108 mg, 4.5 mmol) was added to Phloroglucinol (126 mg, 1 mmol) DMF solution slowly, then tert-butyl(3-chloropropyl)carbamate (935 mg, 4.5 mmol) was added and heated to 55 C. overnight. The resultant solution was diluted in 30 mL ethyl acetate, washed with 20 mL water 4 times. Organic layer was collected, after evaporating the solvent, the residue was further purified with silica gel column to afford 146 mg product 2-1a (24% yield) as a white solid. A mixture of 100 muL TFA and 100 muL dichloromethane was added to 2-1a to remove Boc protection group. All solvents are evaporated off after incubating at room temperature for 2 hr. The triamino derivative 2-1b was directly used without further purification.

The basis of chemical reaction formula synthesis, the synthesis route is composed of some specific reactions and combined according to certain logical thinking. We look forward to the emergence of more reaction modes in the future.

Reference:
Patent; Pacific Biosciences of California, Inc.; Sebo, Lubomir; Hanes, Jeremiah; Shen, Gene; Brogley, Louis; Yue, Stephen; Zheng, Frank; Lapin, Yuri; Lyle, John; Osuna, Honey; Fedorov, Andrei; (184 pag.)US9957291; (2018); B2;,
Amide – Wikipedia,
Amide – an overview | ScienceDirect Topics