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

HRID 1024965
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HRID 1024965 반응식
[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
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참가 물질

4

반응물 2

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

생성물 1

HCID 53628381(3R,5S)-3,5-dimethylpiperazine-1-sulfonamide수율 70%

시약·촉매·용매 1

HCID 312751,4-Dioxane용매2회

실험 절차

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 3d. 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 (1.05 g). A mixture of (3R,5S)-3,5-dimethylpiperazine-1-sulfonamide (0.541 g), tris(dibenzylideneacetone)dipalladium (0) (50 mg), 2-dicyclohexylphosphino-2′,4′,6′-tri-isopropyl-1,1′-biphenyl (XPHOS) (50 mg), cesium carbonate (0.731 g) and (2R,3R)-3-({6-chloro-2-[(2,3-difluorobenzyl)thio]pyrimidin-4-yl}oxy)butan-2-ol ((the product of example 4 step i), 0.541 g) in dioxane (40 mL) was heated at reflux in a microwave at 100° C., 300 W, open vessel with cooling for 20 min. The reaction mixture was then reduced in vacuo and the residue separated between DCM (200 ml) and H2O (200 ml). The organics were separated and the aqueous layer was re-extracted with DCM (2×200 ml). Organics were combined, dried (MgSO4) and reduced in vacuo and the resulting residue was purified by prep HPLC to give the title compound as a white solid. Yield: 80 mg

후처리

  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

출처 및 근거

ORD 기록
ord-692846ed19cc4070afbb641773fa7265
출처 데이터셋
uspto-grants-2014_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08722883B2

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