Triphenylphosphine → 5-(3-((4-Acetyl-3-hydroxy-2-methylphenoxy)methyl)phenylthio) picolinonitrile

HRID 2267062노트

반응식

HRID 2267062 반응식
C1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1.CC(OC(/N=N/C(OC(C)C)=O)=O)C.[OH:34][CH2:35][C:36]1[CH:37]=[C:38]([S:42][C:43]2[CH:44]=[CH:45][C:46]([C:49]#[N:50])=[N:47][CH:48]=2)[CH:39]=[CH:40][CH:41]=1.[OH:51][C:52]1[C:57]([CH3:58])=[C:56](O)[CH:55]=[CH:54][C:53]=1[C:60](=[O:62])[CH3:61]>C1COCC1.C(OCC)(=O)C>[C:60]([C:53]1[CH:54]=[CH:55][C:56]([O:34][CH2:35][C:36]2[CH:37]=[C:38]([S:42][C:43]3[CH:44]=[CH:45][C:46]([C:49]#[N:50])=[N:47][CH:48]=3)[CH:39]=[CH:40][CH:41]=2)=[C:57]([CH3:58])[C:52]=1[OH:51])(=[O:62])[CH3:61]

참가 물질

7

반응물 4

HCID 11776TriphenylphosphineHCID 5921391-(2,4-Dihydroxy-3-methylphenyl)ethan-1-oneHCID 5363146Diisopropyl azodicarboxylateHCID 68535288HCID 68535288, 화합물

생성물 1

HCID 595995135-(3-((4-Acetyl-3-hydroxy-2-methylphenoxy)methyl)phenylthio) picolinonitrile수율 73%

시약·촉매·용매 2

HCID 8028Tetrahydrofuran용매HCID 8857Ethyl Acetate용매

실험 절차

Add triphenylphosphine (1.84 g, 7.02 mmol) and diisopropylazodicarboxylate (1.42 g, 7.02 mmol) to a solution of 5-(3-(hydroxymethyl)phenylthio)picolinonitrile (1.70 g, 7.02 mmol) and 1-(2,4-dihydroxy-3-methylphenyl)ethanone (1.17 g, 7.02 mmol) in THF (35.1 mL). Stir overnight. Dilute with ethyl acetate. Wash the mixture with water and brine. Dry, filter and concentrate to afford the title compound (2.00 g, 73%). Use as is. MS (APCI-neg) m/z (rel intensity): 390 (M+H, 100%).

후처리

  1. washWash the mixture with water and brine
  2. customDry
  3. filtrationfilter
  4. concentrationconcentrate

출처 및 근거

ORD 기록
ord-ef27bc10ad9744f690a660c7106fb1fc
출처 데이터셋
uspto-grants-2010_12
특허 번호
US07858646B2

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