Hydrochloric Acid → HCID 56999634, compound

HRID 1251372Notes

Reaction equation

HRID 1251372 reaction equation
[S:1]1[CH:5]=[CH:4][CH:3]=[C:2]1[C:6]1([NH2:12])[CH2:11][CH2:10][CH2:9][CH2:8][CH2:7]1.[C:13]([O:16]C(=O)C)(=[O:15])[CH3:14].Cl>N1C=CC=CC=1>[C:13]([O:16][NH:12][C:6]1([C:2]2[S:1][CH:5]=[CH:4][CH:3]=2)[CH2:11][CH2:10][CH2:9][CH2:8][CH2:7]1)(=[O:15])[CH3:14]

Participants

5

Reactant 3

HCID 313Hydrochloric AcidHCID 7918Acetic AnhydrideHCID 820723Cyclohexanamine, 1-(2-thienyl)-

Product 1

HCID 56999634HCID 56999634, compound

Reagents, catalysts & solvents 1

HCID 1049PyridineSolvent

Procedure

The amine of Stage 17c (3 g, 16.6 mmoles) in pyridine (100 ml) is introduced into a 250 ml three-necked flask, and acetic anhydride (51 g, 50 mmoles) is added dropwise. After 4 hours under agitation at ambient temperature, 100 ml of an HCl solution (10%) is added and the product formed is extracted with ether (3×50 ml). The organic phase is washed with an HCl solution (10%) (2×80 ml), then with water (2×80 ml), dried over MgSO4 and concentrated to dryness. In this way, a white solid is obtained (3.1 g, 84%).

Workup

  1. customthe product formed
  2. extractionis extracted with ether (3×50 ml)
  3. washThe organic phase is washed with an HCl solution (10%) (2×80 ml)
  4. dry with materialwith water (2×80 ml), dried over MgSO4
  5. concentrationconcentrated to dryness
  6. customIn this way, a white solid is obtained (3.1 g, 84%)

Sources & evidence

ORD record
ord-bde15c589a3a454cbd21913ab34b5dc4
Source dataset
uspto-grants-2002_01
Patent number
US06342511B1

Reaction notes

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