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!

2-(2-CHLORO-ACETYLAMINO)-4,5,6,7-TETRAHYDRO-BENZO[B]THIOPHENE-3-CARBOXYLIC ACID AMIDE synthesis

3synthesis methods
-

Yield:20886-87-7 84%

Reaction Conditions:

with triethylamine at 0 - 20; for 2 h;

Steps:

10 Example 10: r4-('Cvclopropyl-methyl-amino -5,6,7,8-tetrahvdro-benzor4,51thienor2,3- dlpyrimidin-2-vH -methanol (Compound 49)

Example 10: r4-('Cvclopropyl-methyl-amino -5,6,7,8-tetrahvdro-benzor4,51thienor2,3- dlpyrimidin-2-vH -methanol (Compound 49) To a mixture of 2-amino-4,5,6,7-tetrahydro-l-benzothiophene-3-carboxamide (30 g, 0.153 mol) and triethylamine (18.5g, 0.183mol) in DCM (200 ml) was added chloro-acetyl chloride (20.57 g, 0.183 mol) slowly at 0 C, and the resulting mixture was stirred at room temperature for 2h. The reaction mixture was concentrated to half of the volume to afford the solid product which was filtered, washed with 10 ml of DCM and dried to provide 2-(2- chloro-acetylamino)-4,5,6,7-tetrahydro-benzo[b]thiophene-3-carboxylic acid amide (35 g, 84%) as off-white solid. XH NMR (400 MHz, DMSO-d6): δ 1.65-1.75 (m, 4H), 2.58-2.72 (m, 4H), 4.49 (s, 2H), 7.29 (s, 1H), 7.42 (s, 1H), 12.23 (s, 1H); LC-MS: [M+H] = 272.8, 275.1, 257.9 & 255.9 m/z.

References:

WO2013/112651,2013,A2 Location in patent:Page/Page column 64