5-tert-Butoxycarbonylamino-pyridine-2-carboxylic acid methyl ester synthesis
- Product Name:5-tert-Butoxycarbonylamino-pyridine-2-carboxylic acid methyl ester
- CAS Number:131052-40-9
- Molecular formula:C12H16N2O4
- Molecular Weight:252.27
24424-99-5
796 suppliers
$13.50/25G
67515-76-8
129 suppliers
$45.00/500mg
131052-40-9
31 suppliers
$141.38/250mgs:
Yield:131052-40-9 93.2%
Reaction Conditions:
with sodium hexamethyldisilazane in N,N-dimethyl-formamide at -40 - -30;
Steps:
7 Compound II-22 Preparation of Compound III-22
NaHMDS (821.25 ml, 1.643 mol, 2.5 eq) and DMF (400 mL) were added to the reaction flask, and II-22 (100.00 g, 0.657 mol, 1.0 eq) and (Boc)2O (157.61) were added dropwise at -30 to -40°C. g, 0.723mol, 1.1eq)DMF (600 mL) solution was added. LC-MS showed that the reaction of the raw material was complete.Tertiary ether (1L) was added at 30-40°C, and acetic acid (200.00 g) was added dropwise.Methyl tertiary ether (200 mL) mixed solution was added and stirred for 30 minutes.The reaction solution was poured into a saturated aqueous solution of ammonium chloride (3.5 L) and the layers were separated and separated.The aqueous phase is extracted with methyl tert-butyl ether (1L×2) and the organic phases are combined.Washed (500mL x 3), saturated sodium chloride (500mL x 1),Anhydrous sodium sulfate was dried, and the organic phase was evaporated to remove the solvent and petroleum ether (1L) was added.The slurry was suction filtered and dried to give Compound III-22 as an off-white solid, 154.5 g.Yield: 93.2%.
References:
CN107602556,2018,A Location in patent:Paragraph 0115; 0117; 0118
17874-76-9
75 suppliers
$42.41/250mgs:
75-65-0
756 suppliers
$10.00/10ml
131052-40-9
31 suppliers
$141.38/250mgs:
24242-20-4
263 suppliers
$6.00/250mg
131052-40-9
31 suppliers
$141.38/250mgs:
100-26-5
357 suppliers
$8.00/5g
131052-40-9
31 suppliers
$141.38/250mgs: