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Triphenylphosphine → HCID 66558838, 화합물

HRID 1530568
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HRID 1530568 반응식
[CH:1]([N:4]1[C:8]([C:9]2[N:18]=[C:17]3[N:11]([CH2:12][CH2:13][O:14][C:15]4[CH:22]=[C:21]([OH:23])[CH:20]=[CH:19][C:16]=43)[CH:10]=2)=[N:7][C:6]([CH3:24])=[N:5]1)([CH3:3])[CH3:2].[F:25][C:26]1[CH:27]=[N:28][CH:29]=[CH:30][C:31]=1[CH:32](O)[CH3:33].C1C=CC(P(C2C=CC=CC=2)C2C=CC=CC=2)=CC=1.CC(OC(/N=N/C(OC(C)C)=O)=O)C>O1CCOCC1>[F:25][C:26]1[CH:27]=[N:28][CH:29]=[CH:30][C:31]=1[CH:32]([O:23][C:21]1[CH:20]=[CH:19][C:16]2[C:17]3[N:11]([CH:10]=[C:9]([C:8]4[N:4]([CH:1]([CH3:3])[CH3:2])[N:5]=[C:6]([CH3:24])[N:7]=4)[N:18]=3)[CH2:12][CH2:13][O:14][C:15]=2[CH:22]=1)[CH3:33]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 11776TriphenylphosphineHCID 5363146Diisopropyl azodicarboxylateHCID 131295791-(3-Fluoropyridin-4-yl)ethanolHCID 136414067HCID 136414067, 화합물

생성물 1

HCID 66558838HCID 66558838, 화합물

시약·촉매·용매 1

HCID 312751,4-Dioxane용매

실험 절차

To a suspension of 2-(2-isopropyl-5-methyl-2H-[1,2,4]triazol-3-yl)-4,5-dihydro-6-oxa-1,3a-diazabenzo[e]azulen-8-ol (300 mg, 0.92 mmol), 1-(3-fluoropyridin-4-yl)ethanol (195 mg, 1.38 mmol) and PPh3 (411 mg, 1.57 mmol) in dioxane (5 mL) was added DIAD (325 μL, 1.57 mmol) and the resulting yellow solution stirred at RT for 2 h. The reaction mixture was partitioned between EtOAc and 1M NaOH, the organic phase dried (MgSO4) and concentrated in vacuo. The resulting residue was purified by column chromatography (Si-PCC, gradient 0-10% MeOH in EtOAc) then triturated with TBME affording 167 (220 mg, 53%). LCMS: RT 4.36 min [M+H]+ 449.3. 1H NMR (DMSO, 400 MHz): δ 8.47 (1H, d, J=1.61 Hz), 8.39-8.36 (2H, m), 7.56 (1H, s), 7.39-7.34 (1H, m), 6.69 (1H, dd, J=8.99, 2.60 Hz), 6.46 (1H, d, J=2.57 Hz), 5.91-5.83 (1H, m), 5.66 (1H, q, J=6.47 Hz), 4.44-4.43 (2H, m), 4.39-4.35 (2H, m), 2.40 (3H, s), 1.68 (3H, d, J=6.45 Hz), 1.55 (6H, d, J=6.65 Hz)

후처리

  1. customThe reaction mixture was partitioned between EtOAc and 1M NaOH
  2. dry with materialthe organic phase dried (MgSO4)
  3. concentrationconcentrated in vacuo
  4. customThe resulting residue was purified by column chromatography (Si-PCC, gradient 0-10% MeOH in EtOAc)
  5. customthen triturated with TBME affording 167 (220 mg, 53%)

출처 및 근거

ORD 기록
ord-bb577e20f9fa4cbea9b59fe32bc8c86f
출처 데이터셋
uspto-grants-2015_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09090628B2

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