HomeMCPWorkbenchSkills
HomeWorkbenchNotificationsMe
llms.txt · MCP GuidePrivacy Policy · Terms of Service · Supportv1.8.0
  1. Home
  2. /Reaction

Dimethyl Sulfoxide → N-[4-[2-Acetyl-4-(3-methylphenyl)-1,3-thiazol-5-YL]-2-pyridyl]propionamide

HRID 1727378
Notes
Print preview

Reaction equation

HRID 1727378 reaction equation
CS(C)=O.C(Cl)(=O)C(Cl)=O.[OH:11][CH:12]([C:14]1[S:15][C:16]([C:26]2[CH:31]=[CH:30][N:29]=[C:28]([NH:32][C:33](=[O:36])[CH2:34][CH3:35])[CH:27]=2)=[C:17]([C:19]2[CH:24]=[CH:23][CH:22]=[C:21]([CH3:25])[CH:20]=2)[N:18]=1)[CH3:13].C(N(CC)CC)C.C(=O)([O-])O.[Na+]>ClCCl>[C:12]([C:14]1[S:15][C:16]([C:26]2[CH:31]=[CH:30][N:29]=[C:28]([NH:32][C:33](=[O:36])[CH2:34][CH3:35])[CH:27]=2)=[C:17]([C:19]2[CH:24]=[CH:23][CH:22]=[C:21]([CH3:25])[CH:20]=2)[N:18]=1)(=[O:11])[CH3:13]
ParticipantsConditionsProcedureWorkupSources & evidenceReaction notes

Participants

7

Reactant 5

HCID 679Dimethyl SulfoxideHCID 8471TriethylamineHCID 65578Oxalyl chlorideHCID 516892Sodium BicarbonateHCID 53432117N-[4-[2-(1-Hydroxyethyl)-4-(3-methylphenyl)-1,3-thiazol-5-YL]-2-pyridyl]propionamide

Product 1

HCID 53432121
N-[4-[2-Acetyl-4-(3-methylphenyl)-1,3-thiazol-5-YL]-2-pyridyl]propionamide
Yield 60.2%

Reagents, catalysts & solvents 1

HCID 6344DichloromethaneSolvent2×

Conditions

Temperature
-50 °C

Procedure

A solution of dimethylsulfoxide (0.30 mL, 4.2 mmol) in dichloromethane (1.0 mL) was added to a solution of oxalyl chloride (0.11 mL, 1.26 mmol) at −78° C. and the resulting mixture was stirred for 15 minutes. A solution of N-[4-[2-(1-hydroxyethyl)-4-(3-methylphenyl)-1,3-thiazol-5-yl]-2-pyridyl]propionamide (0.38 g, 1.0 mmol) in dichloromethane (1.5 mL) was added to the mixture and the resulting mixture was stirred for 45 minutes. The reaction mixture was allowed to warm up to −50° C. and triethylamine (0.72 mL, 5.17 mmol) was added dropwise to the mixture. The resulting mixture was stirred for 30 minutes and poured into aqueous sodium hydrogen carbonate. The mixture was extracted with ethyl acetate and the extracts were washed with aqueous sodium hydrogen carbonate solution and brine. The resulting solution was dried, and concentrated under reduced pressure. The residue was purified by silica gel column chromatography (hexane-ethyl acetate=2:1) to obtain a crude crystal. The obtained crude crystal was recrystallized from isopropyl ether to give a title compound (0.22 g, yield 58%).

Workup

  1. stirringthe resulting mixture was stirred for 45 minutes
  2. stirringThe resulting mixture was stirred for 30 minutes
  3. extractionThe mixture was extracted with ethyl acetate
  4. washthe extracts were washed with aqueous sodium hydrogen carbonate solution and brine
  5. customThe resulting solution was dried
  6. concentrationconcentrated under reduced pressure
  7. customThe residue was purified by silica gel column chromatography (hexane-ethyl acetate=2:1)
  8. customto obtain a crude crystal
  9. customThe obtained crude crystal
  10. customwas recrystallized from isopropyl ether

Sources & evidence

ORD record
ord-e37c7190c9db48e1a23c2bc1c38db959
Source dataset
uspto-grants-2009_02
DOI
10.6084/m9.figshare.5104873.v1
Patent number
US07495018B2

Reaction notes

Loading…

On this pageParticipantsConditionsProcedureWorkupSources & evidenceReaction notes