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Tetrahydrofuran → HCID 11677831, 화합물

HRID 1811577
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HRID 1811577 반응식
[CH2:1]([CH:3]([O:6][C:7]([N:9]1[CH2:14][CH2:13][CH:12]([O:15][C:16]2[C:21]([O:22][CH3:23])=[C:20](Cl)[N:19]=[CH:18][N:17]=2)[CH2:11][CH2:10]1)=[O:8])[CH2:4][CH3:5])[CH3:2].[CH3:25][S:26]([C:29]1[N:34]=[C:33]([CH3:35])[C:32]([NH2:36])=[CH:31][CH:30]=1)(=[O:28])=[O:27].C(N1CCN2CCN(CC(C)C)P1N(CC(C)C)CC2)C(C)C.CC(C)([O-])C.[K+].C1COCC1>O1CCOCC1.C([O-])(=O)C.[Pd+2].C([O-])(=O)C>[CH2:1]([CH:3]([O:6][C:7]([N:9]1[CH2:14][CH2:13][CH:12]([O:15][C:16]2[C:21]([O:22][CH3:23])=[C:20]([NH:36][C:32]3[C:33]([CH3:35])=[N:34][C:29]([S:26]([CH3:25])(=[O:28])=[O:27])=[CH:30][CH:31]=3)[N:19]=[CH:18][N:17]=2)[CH2:11][CH2:10]1)=[O:8])[CH2:4][CH3:5])[CH3:2]
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참가 물질

8

반응물 5

HCID 8028TetrahydrofuranHCID 45712432,8,9-Triisobutyl-2,5,8,9-tetraaza-1-phosphabicyclo(3.3.3)undecaneHCID 23665647Potassium tert-butoxideHCID 510505272-Methyl-6-(methylsulfonyl)pyridin-3-amineHCID 86606453HCID 86606453, 화합물

생성물 1

HCID 11677831HCID 11677831, 화합물
수율 2.11%

시약·촉매·용매 2

HCID 167845palladium(II) acetate촉매HCID 312751,4-Dioxane용매

반응 조건

온도
100 °C

실험 절차

4-(6-Chloro-5-methoxy-pyrimidin-4-yloxy)-piperidine-1-carboxylic acid 1-ethyl-propyl ester, (0.50 g, 1.40 mmol) and 6-methanesulfonyl-2-methyl-pyridin-3-ylamine (0.26 g, 1.40 mmol) and palladium acetate (0.062 g, 0.28 mmol) and 2,8,9-triisobutyl-2,5,8,9-tetraaza-1-phospha-bicyclo[3.3.3]undecane (0.191 g, 0.559 mmol) were combined in 50 mL dioxane, purged with nitrogen and a 1M solution of potassium t-butoxide in THF (2.79 mL, 2.79 mmol) added dropwise. The reaction was heated to 100° C. and stirred for 2 hours, then was filtered, concentrated, acidified and purified by prep HPLC, the desired fractions partitioned between saturated sodium hydrogen carbonate and ethyl acetate, the organic phase washed with brine and dried with magnesium sulfate to yield (15 mg, 0.029 mmol, 2.11% yield) desired product, as a white solid. 1HNMR (CDCl3, 400 MHz) δ 0.91 (t, J=7.33 Hz, 6H), 1.54-1.64 (m, 4H), 1.77-1.87 (m, 2H), 1.99-2.08 (m, 2H), 2.65 (s, 3H), 3.19 (s, 3H), 3.39-3.46 (m, 2H), 3.78-3.85 (m, 2H), 4.00 (s, 3H), 4.67 (pent, J=6.32 Hz, 1H), 5.36-5.43 (hept, J=3.79 Hz, 1H), 7.31 (bs, 1H), 7.96 (d, J=8.34 Hz, 1H), 8.20 (s, 1H), 9.02 (d, J=8.59 Hz, 1H). Exact mass calculated for C23H33N5O6S: 507.22 found: 508.5 (MH+).

후처리

  1. custompurged with nitrogen
  2. filtrationwas filtered
  3. concentrationconcentrated
  4. custompurified by prep HPLC
  5. customthe desired fractions partitioned between saturated sodium hydrogen carbonate and ethyl acetate
  6. washthe organic phase washed with brine
  7. dry with materialdried with magnesium sulfate

출처 및 근거

ORD 기록
ord-b71767844f084661af093a40344718d8
출처 데이터셋
uspto-grants-2013_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08362248B2

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