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Hydrochloric Acid → Pf-4191834

HRID 501501
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HRID 501501 반응식
Br[C:2]1[CH:7]=[CH:6][C:5]([C:8]2[N:12]([CH3:13])[N:11]=[CH:10][CH:9]=2)=[CH:4][CH:3]=1.C([Si](C(C)C)(C(C)C)[S:18][C:19]1[CH:20]=[C:21]([C:25]2([C:31]([NH2:33])=[O:32])[CH2:30][CH2:29][O:28][CH2:27][CH2:26]2)[CH:22]=[CH:23][CH:24]=1)(C)C.CC(C)([O-])C.[K+].C1COCC1.Cl>CC(O)C.C1C=CC([P]([Pd]([P](C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)([P](C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)[P](C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)=CC=1.O>[CH3:13][N:12]1[C:8]([C:5]2[CH:6]=[CH:7][C:2]([S:18][C:19]3[CH:20]=[C:21]([C:25]4([C:31]([NH2:33])=[O:32])[CH2:30][CH2:29][O:28][CH2:27][CH2:26]4)[CH:22]=[CH:23][CH:24]=3)=[CH:3][CH:4]=2)=[CH:9][CH:10]=[N:11]1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

9

반응물 5

HCID 313Hydrochloric AcidHCID 8028TetrahydrofuranHCID 125810925-(4-Bromophenyl)-1-methyl-1H-pyrazoleHCID 23665647Potassium tert-butoxideHCID 566014104-(3-(triisopropylsilylthio)phenyl)tetrahydro-2H-pyran-4-carboxamide

생성물 1

HCID 24986635Pf-4191834수율 85.9%

시약·촉매·용매 3

HCID 178418397HCID 178418397, 화합물촉매HCID 962Water용매HCID 3776Isopropanol용매

실험 절차

A mixture of 5-(4-bromophenyl)-1-methyl-1H-pyrazole (0.50 g, 2.10 mmols,), 4-{3-[(tri-isopropylsilyl)thio]phenyl}tetrahydro-2H-pyran-4-carboxamide (0.83 g, 2.10 mmols), Tetrakis(triphenylphosphine)palladium(0) (243 mg, 0.10 equivalents), bis[(2-diphenyl-phosphino)]phenyl ether (113 mg, 0.10 equivalents), and 1.0 M potassium tert-butoxide in THF (6.3 mmols, 3 equivalents) in iPrOH (15 mL) that contained 5% water was heated for 4 hours at 90 degrees Celcius in an atmosphere of nitrogen. The reaction mixture was cooled to room temperature and 7 mL of 1N HCl was added. The product was precipitated by the addition of water (30 mL). The precipitate was collected by suction filtration and washed with water (2×20 mL) and cold ethyl ether (4×20 mL). The tan brown solid was dissolved in a small volume of methylene chloride containing 1% methanol and applied to a 140 g cartridge of silica gel. The cartridge was eluted with an acetone:hexane gradient. The appropriate fractions were concentrated and triturated with methanol to produce a white solid (710 mg) as product. 1H NMR (400 MHz, DMSO-d6) δ ppm 1.75-1.84 (m, 3H) 2.40 (d, J=13.54 Hz, 3H) 3.43-3.51 (m, 1H) 3.72 (d, J=11.34 Hz, 3H) 3.84 (s, 3H) 6.40 (d, J=1.46 Hz, 1H) 7.02 (s, 1H) 7.22-7.30 (m, 2H) 7.34 (d, J=8.05 Hz, 1H) 7.38-7.43 (m, 2H) 7.45-7.52 (m, 3H). HRMS calc M+H, 394.1589, found 394.1630.

후처리

  1. temperaturewas heated for 4 hours at 90 degrees Celcius in an atmosphere of nitrogen
  2. customThe product was precipitated by the addition of water (30 mL)
  3. filtrationThe precipitate was collected by suction filtration
  4. washwashed with water (2×20 mL) and cold ethyl ether (4×20 mL)
  5. dissolutionThe tan brown solid was dissolved in a small volume of methylene chloride containing 1% methanol
  6. washThe cartridge was eluted with an acetone
  7. concentrationThe appropriate fractions were concentrated
  8. customtriturated with methanol

출처 및 근거

ORD 기록
ord-28570f8f84ea42e2a1109607d498fa07
출처 데이터셋
uspto-grants-2010_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07772269B2

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