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Triphenylphosphine → HCID 66863232, 화합물

HRID 253057
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HRID 253057 반응식
[Cl:1][C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][C:3]=1[N:8]1[C:12]([C:13]2[CH:18]=[CH:17][C:16]([Cl:19])=[CH:15][CH:14]=2)=[C:11]([OH:20])[C:10]([C:21]([O:23][CH2:24][CH3:25])=[O:22])=[N:9]1.[C:26]1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=C[CH:27]=1.[O:45]1[CH2:50][CH2:49][N:48]([CH2:51][CH2:52]O)[CH2:47][CH2:46]1.N(C(OC(C)C)=O)=NC(OC(C)C)=O>O1CCCC1>[CH2:26]([N:9]1[CH:10]([C:21]([O:23][CH2:24][CH3:25])=[O:22])[C:11]([O:20][CH2:52][CH2:51][N:48]2[CH2:49][CH2:50][O:45][CH2:46][CH2:47]2)=[C:12]([C:13]2[CH:18]=[CH:17][C:16]([Cl:19])=[CH:15][CH:14]=2)[N:8]1[C:3]1[CH:4]=[CH:5][CH:6]=[CH:7][C:2]=1[Cl:1])[CH3:27]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 11776TriphenylphosphineHCID 611632-MorpholinoethanolHCID 75555Diisopropyl diazene-1,2-dicarboxylateHCID 24828929HCID 24828929, 화합물

생성물 1

HCID 66863232HCID 66863232, 화합물수율 100%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran
용매

실험 절차

To a solution of 1-(2-chlorophenyl)-5-(4-chlorophenyl)-3-ethoxycarbonyl-4-hydroxy-1H-pyrazole (200 mg, compound obtained in Reference Example 1 (4)) in tetrahydrofuran (4 mL) was added triphenylphosphine (208 mg) and 2-morpholino-ethanol (96 μL) and the mixture was stirred. Thereto was added dropwise diisopropyl azodicarboxylate (154 μL) at 0° C. under nitrogen-gas atmosphere and the mixture was stirred at room temperature overnight. The reaction mixture was concentrated in vacuo and the crude product was purified by column chromatography on silica gel (solvent: hexane/ethyl acetate=67/33 to 30/70) to obtain ethyl 1-(2-chlorophenyl)-5-(4-chlorophenyl)-3-ethoxycarbonyl-4-(2-morpholinoethoxy)-1H-pyrazole (463 mg, yield: 100%) as a colorless viscidity.

후처리

  1. stirringthe mixture was stirred at room temperature overnight
  2. concentrationThe reaction mixture was concentrated in vacuo
  3. customthe crude product was purified by column chromatography on silica gel (solvent: hexane/ethyl acetate=67/33 to 30/70)

출처 및 근거

ORD 기록
ord-28bd15e72d1244309d6a7d84390d328b
출처 데이터셋
uspto-grants-2011_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07872006B2

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