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Potassium Acetate → 3-Methyl-3-(4-(4,4,5,5-tetramethyl-1,3,2-dioxaborolan-2-yl)phenyl)thietane 1,1-dioxide

HRID 929261
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HRID 929261 반응식
[BH:1]([O:3]BO)[OH:2].O[C:7]([C:10](O)([CH3:12])[CH3:11])([CH3:9])[CH3:8].C([O-])(=O)C.[K+].Br[C:20]1[CH:25]=[CH:24][C:23]([C:26]2([CH3:32])[CH2:29][S:28](=[O:31])(=[O:30])[CH2:27]2)=[CH:22][CH:21]=1>CN(C=O)C.C1C=CC(P(C2C=CC=CC=2)[C-]2C=CC=C2)=CC=1.C1C=CC(P(C2C=CC=CC=2)[C-]2C=CC=C2)=CC=1.Cl[Pd]Cl.[Fe+2].C(Cl)Cl>[CH3:32][C:26]1([C:23]2[CH:24]=[CH:25][C:20]([B:1]3[O:3][C:10]([CH3:12])([CH3:11])[C:7]([CH3:9])([CH3:8])[O:2]3)=[CH:21][CH:22]=2)[CH2:29][S:28](=[O:31])(=[O:30])[CH2:27]1
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6

반응물 3

HCID 517044Potassium AcetateHCID 124571823-(4-Bromophenyl)-3-methylthietane 1,1-dioxideHCID 178459140HCID 178459140, 화합물

생성물 1

HCID 900421873-Methyl-3-(4-(4,4,5,5-tetramethyl-1,3,2-dioxaborolan-2-yl)phenyl)thietane 1,1-dioxide

시약·촉매·용매 2

HCID 178418807HCID 178418807, 화합물촉매
HCID 6228
Dimethylformamide
용매

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온도
90 °C

실험 절차

Step D To pinacol diboronate (250 mg, 0.986 mmol), potassium acetate (242 mg, 2.466 mmol) and PdCl2(dppf)-CH2Cl2 adduct (67 mg, 0.082 mmol) in a thick-walled tube was added a solution of 3-(4-bromophenyl)-3-methylthietane 1,1-dioxide (226 mg, from Step C) in DMF (5 ml). The tube was flushed with N2, then capped and heated to 90° C. for 4 hours. Then the reaction was cooled to RT and diluted with EtOAc (30 ml) and water (20 ml). The aqueous layer was separated and extracted with EtOAc (25 ml). The combined organic layers were washed with water (50 ml), dried (Na2SO4), filtered and concentrated. The resulting crude material was purified by Isco™ system, 40 g gold cartridge, 40 ml flow rate, gradient—0/100 (1 min) to 50/50 (19 min) to 50/50 (21 min—total run time) of EtOAc/hexanes. The fractions containing the product were combined and concentrated to provide 3-methyl-3-(4-(4,4,5,5-tetramethyl-1,3,2-dioxaborolan-2-yl)phenyl)thietane 1,1-dioxide as a white solid.

후처리

  1. customThe tube was flushed with N2
  2. customcapped
  3. temperatureThen the reaction was cooled to RT
  4. additiondiluted with EtOAc (30 ml) and water (20 ml)
  5. customThe aqueous layer was separated
  6. extractionextracted with EtOAc (25 ml)
  7. washThe combined organic layers were washed with water (50 ml)
  8. dry with materialdried (Na2SO4)
  9. filtrationfiltered
  10. concentrationconcentrated
  11. customThe resulting crude material was purified by Isco™ system, 40 g gold cartridge, 40 ml flow rate, gradient—0/100 (1 min) to 50/50 (19 min) to 50/50 (21 min—total run time) of EtOAc/hexanes
  12. additionThe fractions containing the product
  13. concentrationconcentrated

출처 및 근거

ORD 기록
ord-a768ca25f8bc4002b5a65b7cd1c0aca4
출처 데이터셋
uspto-grants-2016_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09290517B2

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