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Lithium hydroxide, monohydrate → HCID 118875502, 화합물

HRID 60468
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HRID 60468 반응식
C([O:3][CH2:4][CH2:5][CH2:6][N:7]1[C:12](=[O:13])[C:11]2[C:14]([CH2:28][C:29]3[CH:34]=[CH:33][CH:32]=[CH:31][CH:30]=3)=[C:15]([O:18][C:19]3[CH:24]=[CH:23][CH:22]=[C:21]([CH:25]([CH3:27])[CH3:26])[CH:20]=3)[CH:16]=[N:17][C:10]=2[N:9]([CH3:35])[C:8]1=[O:36])=O.O[Li].O>C1COCC1.O.CC(=O)OCC>[CH2:28]([C:14]1[C:11]2[C:12](=[O:13])[N:7]([CH2:6][CH2:5][CH2:4][OH:3])[C:8](=[O:36])[N:9]([CH3:35])[C:10]=2[N:17]=[CH:16][C:15]=1[O:18][C:19]1[CH:24]=[CH:23][CH:22]=[C:21]([CH:25]([CH3:27])[CH3:26])[CH:20]=1)[C:29]1[CH:34]=[CH:33][CH:32]=[CH:31][CH:30]=1
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참가 물질

6

반응물 2

HCID 168937Lithium hydroxide, monohydrateHCID 118875475HCID 118875475, 화합물

생성물 1

HCID 118875502HCID 118875502, 화합물수율 45%

시약·촉매·용매 3

HCID 962Water용매2회HCID 8028Tetrahydrofuran용매HCID 8857Ethyl Acetate
용매

실험 절차

To a solution of 3-(5-benzyl-6-(3-isopropylphenoxy)-1-methyl-2,4-dioxo-1,2-dihydropyrido[2,3-d]pyrimidin-3(4H)-yl)propyl formate (50 mg, 0.10 mmol) in THF (3 ml) and water (3 mL) was added LiOH.H2O (10 mg, 0.20 mmol). The reaction was stirred at RT for 15 min then diluted with EA (30 mL) and water (30 mL). The organic layer was dried over Na2SO4 and concentrated to give a residue which was purified by Prep HPLC to give 5-benzyl-3-(3-hydroxypropyl)-6-(3-isopropyl phenoxy)-1-methylpyrido[2,3-d]pyrimidine-2,4(1H,3H)-dione (15 mg, 45% yield) as a solid. 1H NMR (CDCl3) δ: 8.32 (s, 1H), 7.29 (s, 2H), 7.25-7.12 (m, 4H), 6.99 (d, J=7.9 Hz, 1H), 6.76 (s, 1H), 6.68 (dd, J=8.0, 2.3 Hz, 1H), 4.80 (s, 2H), 4.24 (t, J=6.0 Hz, 2H), 3.70 (s, 3H), 3.52 (dd, J=11.8, 6.2 Hz, 2H), 3.10 (t, J=7.0 Hz, 1H), 2.85 (dt, J=13.9, 6.9 Hz, 1H), 1.98-1.83 (m, 2H), 1.22 (d, J=6.9 Hz, 6H). LCMS: MH+ 460 and TR=3.376 min.

후처리

  1. dry with materialThe organic layer was dried over Na2SO4
  2. concentrationconcentrated
  3. customto give a residue which
  4. customwas purified by Prep HPLC

출처 및 근거

ORD 기록
ord-f6d6ca5196c74a809c3463f4e18c3cc2
출처 데이터셋
uspto-grants-2016_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09440972B2

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