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Methyl 2-methylfuran-3-carboxylate → 2-Methylfuran-3-carboxamide

HRID 339405
Notes
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Reaction equation

HRID 339405 reaction equation
[CH3:1][C:2]1[O:3][CH:4]=[CH:5][C:6]=1[CH2:7][NH2:8].CC1[O:11]C=CC=1C(OC)=O.C[O-].[Na+]>C(N)=O>[CH3:1][C:2]1[O:3][CH:4]=[CH:5][C:6]=1[C:7]([NH2:8])=[O:11]
ParticipantsProcedureWorkupSources & evidenceReaction notes

Participants

5

Reactant 3

HCID 80237Methyl 2-methylfuran-3-carboxylateHCID 10942334Sodium MethoxideHCID 185258661-(2-Methylfuran-3-yl)methanamine

Product 1

HCID 107729742-Methylfuran-3-carboxamideYield 83%

Reagents, catalysts & solvents 1

HCID 713FormamideSolvent

Procedure

(2-Methylfuran-3-yl)methanamine: A solution of 10 mmol (1.256 ml) of methyl 2-methylfuran-3-carboxylate and 38.9 mmol (2.1 g) of NaOMe in 20 ml of formamide was stirred at 100° C. for 30 min. The reaction mixture was poured into ice-water (20 ml) and extracted with ethyl acetate (3×). The extract was dried over MgSO4 and concentrated to give 1.05 g (83%) of 2-methylfuran-3-carboxamide as oil (m/e=126.2 [M+1]). The amide was dissolved in dry THF (10 ml) and drop-wise added to 15 ml of 1M LiAlH4 with 15 ml THF at 0° C. under argon. Then the mixture was stirred for 5 hrs at 60° C. Following cooling, 50% aqueous THF (30 ml) was added to the mixture at 5-10° C. The resulting precipitate was removed by filtration and the filtered solution was dried and concentrated to give an oily product (0.93 g, 84%).

Workup

  1. extractionextracted with ethyl acetate (3×)
  2. dry with materialThe extract was dried over MgSO4
  3. concentrationconcentrated

Sources & evidence

ORD record
ord-26d6b62696d244cc975ac50e37f62d62
Source dataset
uspto-grants-2014_11
DOI
10.6084/m9.figshare.5104873.v1
Patent number
US08895050B2

Reaction notes

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On this pageParticipantsProcedureWorkupSources & evidenceReaction notes