Triphenylphosphine → HCID 68529647, 화합물

HRID 1253771

반응식

HRID 1253771 반응식
[Cl:1][C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][C:3]=1[CH:8]([O:10][C:11](=[O:29])[NH:12][C:13]1[C:14]([CH3:28])=[N:15][O:16][C:17]=1[C:18]1[CH:23]=[CH:22][C:21]([C:24]#[C:25][CH2:26]O)=[CH:20][CH:19]=1)[CH3:9].[F:30][C:31]([F:43])([F:42])[C:32]1[NH:36][N:35]=[CH:34][C:33]=1[C:37]([O:39][CH2:40][CH3:41])=[O:38].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>[CH2:40]([O:39][C:37]([C:33]1[CH:34]=[N:35][N:36]([CH2:26][C:25]#[C:24][C:21]2[CH:22]=[CH:23][C:18]([C:17]3[O:16][N:15]=[C:14]([CH3:28])[C:13]=3[NH:12][C:11]([O:10][CH:8]([C:3]3[CH:4]=[CH:5][CH:6]=[CH:7][C:2]=3[Cl:1])[CH3:9])=[O:29])=[CH:19][CH:20]=2)[C:32]=1[C:31]([F:30])([F:42])[F:43])=[O:38])[CH3:41]

참가 물질

6

반응물 4

HCID 11776TriphenylphosphineHCID 75555Diisopropyl diazene-1,2-dicarboxylateHCID 596095Ethyl 3-(Trifluoromethyl)pyrazole-4-carboxylateHCID 70878238HCID 70878238, 화합물

생성물 1

HCID 68529647HCID 68529647, 화합물

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

To a solution of {5-[4-(3-hydroxy-prop-1-ynyl)-phenyl]-3-methyl-isoxazol-4-yl}-carbamic acid 1-(2-chloro-phenyl)-ethyl ester (0.200 g, 0.49 mmol), ethyl 5-(trifluoromethyl)-1H-pyrazole-4-carboxylate (0.101 g, 0.49 mmol), and triphenylphosphine (0.127 g, 0.49 mmol) in THF (4 mL) was added diisopropyl azodicarboxylate (0.10 mL, 0.49 mmol), and the reaction was stirred at room temperature for 2 hours. The mixture was concentrated, and the residue was purified by preparative HPLC to give the title compound.

후처리

  1. concentrationThe mixture was concentrated
  2. customthe residue was purified by preparative HPLC

출처 및 근거

ORD 기록
ord-3f35ad9b07114f939008e9fd17412984
출처 데이터셋
uspto-grants-2013_06
특허 번호
US08455499B2

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