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Triphenylphosphine → HCID 66892278, 화합물

HRID 456230
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HRID 456230 반응식
[CH3:1][O:2][C:3](=[O:25])[CH2:4][C:5]1[CH:6]=[C:7]([C:13]2[CH:18]=[CH:17][C:16]([C:19]([F:22])([F:21])[F:20])=[CH:15][C:14]=2[CH2:23]O)[C:8]([O:11][CH3:12])=[CH:9][CH:10]=1.[CH3:26][C:27]1([C:34]2[CH:39]=[CH:38][CH:37]=[CH:36][CH:35]=2)[NH:31][C:30](=[O:32])[NH:29][C:28]1=[O:33].C1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1.N(C(OC(C)C)=O)=NC(OC(C)C)=O>C1COCC1>[CH3:1][O:2][C:3](=[O:25])[CH2:4][C:5]1[CH:6]=[C:7]([C:13]2[CH:18]=[CH:17][C:16]([C:19]([F:21])([F:22])[F:20])=[CH:15][C:14]=2[CH2:23][N:29]2[C:28](=[O:33])[C:27]([CH3:26])([C:34]3[CH:35]=[CH:36][CH:37]=[CH:38][CH:39]=3)[NH:31][C:30]2=[O:32])[C:8]([O:11][CH3:12])=[CH:9][CH:10]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 11776TriphenylphosphineHCID 75555Diisopropyl diazene-1,2-dicarboxylateHCID 930435-Methyl-5-phenylhydantoinHCID 66606415(2'-Hydroxymethyl-6-methoxy-4'-trifluoromethyl-biphenyl-3-yl)-acetic acid methyl ester

생성물 1

HCID 66892278HCID 66892278, 화합물

시약·촉매·용매 1

HCID 8028
Tetrahydrofuran
용매

실험 절차

To (2′-hydroxymethyl-6-methoxy-4′-trifluoromethyl-biphenyl-3-yl)-acetic acid methyl ester (0.158 g, 0.44 mmol), 5-methyl-5-phenylhydantoin (0.102 g, 0.53 mmol), and triphenylphosphine (0.141 g, 0.53 mmol) in THF (3 mL) was added diisopropyl azodicarboxylate (0.1 mL, 0.53 mmol), and the reaction was stirred overnight at room temperature. Once no starting material was seen by analytical LCMS, the mixture was concentrated and purified by silica gel chromatography (0-50% EtOAc in hexanes) to give the title compound.

후처리

  1. concentrationthe mixture was concentrated
  2. custompurified by silica gel chromatography (0-50% EtOAc in hexanes)

출처 및 근거

ORD 기록
ord-c43cced59fb3423db08d157c1b1eb10e
출처 데이터셋
uspto-grants-2013_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08497381B2

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