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Sulfamide → (3R,5S)-3,5-dimethylpiperazine-1-sulfonamide

HRID 1175465
Notes
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Reaction equation

HRID 1175465 reaction equation
[CH3:1][C@@H:2]1[CH2:7][NH:6][CH2:5][C@H:4]([CH3:8])[NH:3]1.[S:9](N)([NH2:12])(=[O:11])=[O:10]>O1CCOCC1>[CH3:8][C@H:4]1[NH:3][C@@H:2]([CH3:1])[CH2:7][N:6]([S:9]([NH2:12])(=[O:11])=[O:10])[CH2:5]1
ParticipantsProcedureWorkupSources & evidenceReaction notes

Participants

4

Reactant 2

HCID 82267SulfamideHCID 6950261rel-(2R,6S)-2,6-dimethylpiperazine

Product 1

HCID 53628381(3R,5S)-3,5-dimethylpiperazine-1-sulfonamideYield 19.3%

Reagents, catalysts & solvents 1

HCID 312751,4-DioxaneSolvent2×

Procedure

To a solution of (2R,6S)-2,6-dimethylpiperazine (1 g) in dioxane (10 ml) was added sulfamide (0.746 g) and the reaction mixture was then heated at reflux in dioxane for 72 h. The reaction mixture was partitioned between EtOAc (150 ml) and H2O (150 ml) and the aqueous re-extracted with EtOAc (2×150 ml). Organics were collected dried and reduced in vacuo to yield (3R,5S)-3,5-dimethylpiperazine-1-sulfonamide as a white solid (0.29 g). A mixture of (3R,5S)-3,5-dimethylpiperazine-1-sulfonamide (0.29 g), tris(dibenzylideneacetone)dipalladium (0) (50 mg), 2-dicyclohexylphosphino-2′,4′,6′-tri-isopropyl-1,1′-biphenyl (XPHOS) (50 mg), cesium carbonate (0.628 g) and 2-[[6-chloro-2-[[(2,3-difluorophenyl)methyl]thio]-4-pyrimidinyl]oxy]-(2R)-propanoic acid ethyl ester (the product of example 5 step i), 0.5 g) in dioxane (10 mL) was heated at reflux in a microwave at 100° C., 300 W, open vessel with cooling for 30 min. The reaction mixture was then reduced in vacuo and the residue was partitioned between EtOAc (150 ml) and H2O (100 ml). The organics were separated and the aqueous layer was re-extracted with EtOAc (2×150 ml). Organics were combined, dried (MgSO4) and reduced in vacuo to give the subtitle compound as a yellow solid. Yield: 0.940 g

Workup

  1. temperaturethe reaction mixture was then heated
  2. customThe reaction mixture was partitioned between EtOAc (150 ml) and H2O (150 ml)
  3. extractionthe aqueous re-extracted with EtOAc (2×150 ml)
  4. customOrganics were collected
  5. customdried

Sources & evidence

ORD record
ord-8ebdbd714b00482b8efe1d1664fea4fb
Source dataset
uspto-grants-2010_11
DOI
10.6084/m9.figshare.5104873.v1
Patent number
US07838675B2

Reaction notes

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On this pageParticipantsProcedureWorkupSources & evidenceReaction notes