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Nitrogen → HCID 86709516, 화합물

HRID 1501819
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HRID 1501819 반응식
[OH:1][CH:2]1[C:6]2([CH2:11][CH2:10][N:9]([C:12]([O:14][C:15]([CH3:18])([CH3:17])[CH3:16])=[O:13])[CH2:8][CH2:7]2)[C:5](=[O:19])[NH:4][CH:3]1[CH3:20].C[C:22]1([CH3:62])[C:48]2[C:43](=C(P(C3C=CC=CC=3)C3C=CC=CC=3)C=CC=2)[O:42]C2C(P(C3C=CC=CC=3)C3C=CC=CC=3)=CC=CC1=2.C([O-])([O-])=[O:64].[K+].[K+].N#N.O>CC([O-])=O.CC([O-])=O.[Pd+2].O1CCOCC1>[OH:1][CH:2]1[C:6]2([CH2:7][CH2:8][N:9]([C:12]([O:14][C:15]([CH3:16])([CH3:18])[CH3:17])=[O:13])[CH2:10][CH2:11]2)[C:5](=[O:19])[N:4]([C:22]2[CH2:62][O:42][C:43](=[O:64])[CH:48]=2)[CH:3]1[CH3:20]
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

8

반응물 5

HCID 947NitrogenHCID 962WaterHCID 11430Potassium CarbonateHCID 6360441,1'-(9,9-Dimethyl-9H-xanthene-4,5-diyl)bis(1,1-diphenylphosphine)HCID 86709515HCID 86709515, 화합물

생성물 1

HCID 86709516HCID 86709516, 화합물

시약·촉매·용매 2

HCID 167845
palladium(II) acetate
촉매
HCID 312751,4-Dioxane용매

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온도
90 °C

실험 절차

To a round bottom flask was charged tert-butyl 4-hydroxy-3-methyl-1-oxo-2,8-diazaspiro[4.5]decane-8-carboxylate (1000 mg, 3.52 mmol), 4-bromofuran-2(514)-one (860 mg, 5.28 mmol), Pd(OAc)2 (79 mg, 0.352 mmol), Xantphos (305 mg, 0.528 mmol), and K2CO3 (972 mg, 7.03 mmol). The flask was sealed, vacuumed and back filled with N2 and filled with dioxane (14 mL) and water (190 μL, 10.6 mmol). The reaction mixture was heated at 90° C. overnight, and filtered through CELITE®. The filtrate was evaporated to give the crude product, which was purified by column chromatography (0-10% MeOH/DCM, came out at 6% MeOH/DCM, followed by another column with 0-100% EtOAc/hex) to give the title compound. LCMS: [(M+1)]+=367

후처리

  1. customThe flask was sealed
  2. filtrationfiltered through CELITE®
  3. customThe filtrate was evaporated
  4. customto give the crude product, which
  5. customwas purified by column chromatography (0-10% MeOH/DCM

출처 및 근거

ORD 기록
ord-7b676f9819c94b79bc51438c61455690
출처 데이터셋
uspto-grants-2015_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09206198B2

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