Triphenylphosphine → HCID 86604655, 화합물

HRID 1593548노트

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HRID 1593548 반응식
[Cl:1][C:2]1[CH:3]=[C:4]2[C:9](=[CH:10][C:11]=1[O:12][CH2:13][CH2:14][CH2:15][OH:16])[O:8][C:7]([CH3:18])([CH3:17])[CH:6]=[C:5]2[C:19]([F:22])([F:21])[F:20].O[C:24]1[CH:38]=[CH:37][C:27]([O:28][C@@:29]([CH3:36])([CH2:34][CH3:35])[C:30]([O:32][CH3:33])=[O:31])=[CH:26][CH:25]=1.C1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1.N(C(OCC)=O)=NC(OCC)=O>C1COCC1>[Cl:1][C:2]1[CH:3]=[C:4]2[C:9](=[CH:10][C:11]=1[O:12][CH2:13][CH2:14][CH2:15][O:16][C:24]1[CH:38]=[CH:37][C:27]([O:28][C@@:29]([CH3:36])([CH2:34][CH3:35])[C:30]([O:32][CH3:33])=[O:31])=[CH:26][CH:25]=1)[O:8][C:7]([CH3:18])([CH3:17])[CH:6]=[C:5]2[C:19]([F:20])([F:22])[F:21]

참가 물질

6

반응물 4

HCID 11776TriphenylphosphineHCID 220568ethyl N-ethoxycarbonyliminocarbamateHCID 11996320(2S)-Methyl 2-(4-hydroxyphenoxy)-2-methylbutanoateHCID 68565082HCID 68565082, 화합물

생성물 1

HCID 86604655HCID 86604655, 화합물수율 61%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

To a solution of 3-((6-chloro-2,2-dimethyl-4-(trifluoromethyl)-2H-chromen-7-yl)oxy)propan-1-ol (0.5 g, 1.48 mmol), (2S)-Methyl 2-(4-hydroxyphenoxy)-2-methylbutanoate (0.35 g, 1.56 mmol), and triphenylphosphine (0.42 g, 1.6 mmol) in THF (20 mL) was added diethyl azodicarboxylate (0.28 g, 1.6 mmol) and the solution stirred at ambient temperature for 16 h. After concentrating under reduced pressure, the residue thus obtained was chromatographed over silica gel using AcOEt/hexanes to furnish the desired compound (0.49 g).

후처리

  1. concentrationAfter concentrating under reduced pressure
  2. customthe residue thus obtained
  3. customwas chromatographed over silica gel

출처 및 근거

ORD 기록
ord-a10bcdb3089840468c2930b41e0f2cb3
출처 데이터셋
uspto-grants-2007_11
특허 번호
US07297715B2

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