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Sodium Bicarbonate → HCID 50915115, 화합물

HRID 2386216
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HRID 2386216 반응식
Cl[C:2]1[N:11]=[CH:10][C:9]2[N:8]([CH2:12][CH:13]3[CH2:15][CH2:14]3)[C:7](=[O:16])[C:6]3([CH3:21])[CH2:17][O:18][CH2:19][CH2:20][N:5]3[C:4]=2[N:3]=1.[CH3:22][NH:23][C:24]([NH:26][C:27]1[CH:32]=[CH:31][C:30](B2OC(C)(C)C(C)(C)O2)=[CH:29][CH:28]=1)=[O:25].C([O-])(O)=O.[Na+].O.C(#N)C>O.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].CC(O)=O.O1CCOCC1>[CH:13]1([CH2:12][N:8]2[C:7](=[O:16])[C:6]3([CH3:21])[CH2:17][O:18][CH2:19][CH2:20][N:5]3[C:4]3[N:3]=[C:2]([C:30]4[CH:29]=[CH:28][C:27]([NH:26][C:24]([NH:23][CH3:22])=[O:25])=[CH:32][CH:31]=4)[N:11]=[CH:10][C:9]2=3)[CH2:15][CH2:14]1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

9

반응물 4

HCID 516892Sodium BicarbonateHCID 177502733-Methyl-1-[4-(tetramethyl-1,3,2-dioxaborolan-2-yl)phenyl]ureaHCID 18373917Acetonitrile--water (1/1)HCID 86651562HCID 86651562, 화합물

생성물 1

HCID 50915115HCID 50915115, 화합물수율 44.9%

시약·촉매·용매 4

HCID 44119782
Bis(cyclopenta-1,4-dien-1-yl(diphenyl)phosphane);dichloropalladium;iron(2+)
촉매
HCID 176Acetic Acid용매
HCID 962Water용매2회
HCID 312751,4-Dioxane용매

실험 절차

To a microwave vial equipped with a magnetic stirrer was added 2-chloro-5-(cyclopropylmethyl)-6a-methyl-6a,7,9,10-tetrahydro-[1,4]oxazino[3,4-h]pteridin-6(5H)-one (88 mg, 0.285 mmol), 1,4-dioxane (2 ml), 1-methyl-3-(4-(4,4,5,5-tetramethyl-1,3,2-dioxaborolan-2-yl)phenyl)urea (118 mg, 0.428 mmol), NaHCO3 (saturated, 0.491 mL), and PdCl2(dppf) (209 mg, 0.285 mmol). The reaction was irradiated in the microwave at 100° C. for 40 min. The reaction solution was then poured into water, extracted with ethyl acetate three times and the combined organic layers were washed with water and then brine, then dried with Na2SO4, filtered, and the filtrate concentrated in-vacuo to give a brown residue. The aqueous layer was acidified with AcOH (pH about 5) and concentrated in-vacuo to give a grey residue. The combined residues were purified via preparative LC/MS (45-50% gradient of 10 mmol NH4HCO3 in 20/80(v/v) water/acetonitrile in 10 mmol NH4HCO3 in water, Phenomenex Gemini 5 μm C18, 75×30 mm column to give the title compound (54 mg, 0.128 mmol, 44.8% yield) as a white solid. 1H NMR (400 MHz, DMSO-d6) δ ppm 0.25-0.57 (m, 4H) 1.18 (m, 1H) 1.35 (s, 3H) 2.62-2.71 (m, 3H) 3.17-3.26 (m, 1H) 3.54-3.65 (m, 1H) 3.68 (d, J=11.62 Hz, 1H) 3.81 (dd, J=14.53, 6.95 Hz, 1H) 3.89-4.02 (m, 2H) 4.07 (dd, J=11.62, 3.54 Hz, 1H) 4.20 (dd, J=13.77, 2.40 Hz, 1H) 6.07 (d, J=4.80 Hz, 1H) 7.49 (d, J=8.84 Hz, 2H) 8.19 (d, J=8.84 Hz, 2 H) 8.36 (s, 1H) 8.72 (s, 1H). MS [M+H] found 423.

후처리

  1. customTo a microwave vial equipped with a magnetic stirrer
  2. customThe reaction was irradiated in the microwave at 100° C. for 40 min
  3. extractionextracted with ethyl acetate three times
  4. washthe combined organic layers were washed with water
  5. dry with materialbrine, then dried with Na2SO4
  6. filtrationfiltered
  7. concentrationthe filtrate concentrated in-vacuo
  8. customto give a brown residue
  9. concentrationconcentrated in-vacuo
  10. customto give a grey residue

출처 및 근거

ORD 기록
ord-9bd79cb9215548fd98b9bcb663e277ad
출처 데이터셋
uspto-grants-2012_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08268819B2

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