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Benzyl chloroformate → Benzyl[3-(aminocarbonyl)-2-thienyl]carbamate

HRID 385693
Notes
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Reaction equation

HRID 385693 reaction equation
[NH2:1][C:2]1[S:3][CH:4]=[CH:5][C:6]=1[C:7]([NH2:9])=[O:8].C(N(C(C)C)CC)(C)C.[CH2:19]([O:26][C:27](Cl)=[O:28])[C:20]1[CH:25]=[CH:24][CH:23]=[CH:22][CH:21]=1>O1CCCC1>[CH2:19]([O:26][C:27](=[O:28])[NH:1][C:2]1[S:3][CH:4]=[CH:5][C:6]=1[C:7]([NH2:9])=[O:8])[C:20]1[CH:25]=[CH:24][CH:23]=[CH:22][CH:21]=1
ParticipantsProcedureWorkupSources & evidenceReaction notes

Participants

5

Reactant 3

HCID 10387Benzyl chloroformate2×HCID 81531Diisopropylethylamine2×HCID 6994952-Aminothiophene-3-carboxamide

Product 1

HCID 59525796Benzyl[3-(aminocarbonyl)-2-thienyl]carbamate

Reagents, catalysts & solvents 1

HCID 8028TetrahydrofuranSolvent

Procedure

To a stirred solution of 2-aminothiophene-3-carboxamide (5 g, 35.2 mmol) in tetrahydrofuran (200 mL) under argon was added diisopropylethylamine (9.52 ml, 54.5 mmol) and benzyloxycarbonyl chloride (7.53 mL, 52.8 mmol). After stirring for 60 hours, more diisopropylethylamine (9.52 mL, 54.5 mmol) and benzyloxycarbonyl chloride (7.53 mL, 52.8 mmol) were added. After an additional 24 hours, the suspension was filtered and the resulting solution was concentrated to ˜30 mL and diluted with ethyl acetate (100 mL) The organic layer was washed sequentially with saturated aqueous sodium bicarbonate (3×40 mL), a 3:1 mixture of saturated aqueous sodium bicarbonate and water (40 mL), and brine (40 mL), dried with sodium sulfate, filtered, and concentrated. The resulting mixture of white solid and brown oil was triturated with a mixture of ethyl acetate (10 mL) and hexanes (10 mL), and then the solid was collected by filtration. Drying under vacuum afforded the title compound as a solid.

Workup

  1. waitAfter an additional 24 hours
  2. filtrationthe suspension was filtered
  3. concentrationthe resulting solution was concentrated to ˜30 mL
  4. additiondiluted with ethyl acetate (100 mL) The organic layer
  5. washwas washed sequentially with saturated aqueous sodium bicarbonate (3×40 mL)
  6. additiona 3:1 mixture of saturated aqueous sodium bicarbonate and water (40 mL), and brine (40 mL)
  7. dry with materialdried with sodium sulfate
  8. filtrationfiltered
  9. concentrationconcentrated
  10. additionThe resulting mixture of white solid and brown oil
  11. customwas triturated with a mixture of ethyl acetate (10 mL) and hexanes (10 mL)
  12. filtrationthe solid was collected by filtration
  13. customDrying under vacuum

Sources & evidence

ORD record
ord-3146de68c0dd4163b51c04c2f371fd83
Source dataset
uspto-grants-2013_02
DOI
10.6084/m9.figshare.5104873.v1
Patent number
US08367706B2

Reaction notes

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On this pageParticipantsProcedureWorkupSources & evidenceReaction notes