Triphenylphosphine → HCID 67824263, 화합물

HRID 1728270노트

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HRID 1728270 반응식
[CH2:1]([O:4][CH2:5][CH2:6][CH2:7][CH2:8][CH2:9][C:10]1[CH:15]=[CH:14][C:13]([C:16]2[N:21]=[CH:20][C:19]([OH:22])=[CH:18][N:17]=2)=[CH:12][CH:11]=1)[CH2:2][CH3:3].[CH2:23](O)[CH2:24]/[CH:25]=[CH:26]\[CH2:27][CH2:28][CH2:29][CH3:30].N(C(OCC)=O)=NC(OCC)=O.C1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1>O1CCCC1>[CH2:1]([O:4][CH2:5][CH2:6][CH2:7][CH2:8][CH2:9][C:10]1[CH:15]=[CH:14][C:13]([C:16]2[N:21]=[CH:20][C:19]([O:22][CH2:23][CH2:24]/[CH:25]=[CH:26]\[CH2:27][CH2:28][CH2:29][CH3:30])=[CH:18][N:17]=2)=[CH:12][CH:11]=1)[CH2:2][CH3:3]

참가 물질

6

반응물 4

HCID 11776TriphenylphosphineHCID 220568ethyl N-ethoxycarbonyliminocarbamateHCID 53645193-Octen-1-ol, (3Z)-HCID 190171892-[4-(5-[Propyloxy]-1-pentyl)phenyl]-5-hydroxypyrimidine

생성물 1

HCID 67824263HCID 67824263, 화합물

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

A mixture of 0.5 g of 2-[4-(5-[propyloxy]-1-pentyl)phenyl]-5-hydroxypyrimidine, 0.3 g of (Z)-3-octen-1-ol, 0.4 g of diethyl azodicarboxylate, 0.6 g of triphenylphosphine and 25 ml of absolute tetrahydrofuran was stirred at room temperature overnight and then concentrated. The residue was suspended with 50 ml of hot hexane and filtered. The filtrate was concentrated. Chromatography of the residue on silica gel with toluene/hexane (vol. 1:1) and recrystallization from methanol gave pure 2-[4-(5-[propyloxy]-1-pentyl)phenyl]-5-([(Z)-3-octenyl]oxy)pyrimidine, m.p. (C-I) 38° C.

후처리

  1. concentrationconcentrated
  2. filtrationfiltered
  3. concentrationThe filtrate was concentrated
  4. customChromatography of the residue on silica gel with toluene/hexane (vol. 1:1) and recrystallization from methanol

출처 및 근거

ORD 기록
ord-fc01e8eeb335460ebfb2623ae924a12d
출처 데이터셋
uspto-grants-1994_07
특허 번호
US05326497

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