Triphenylphosphine → HCID 9906959, 화합물

HRID 991015노트

반응식

HRID 991015 반응식
[NH:1]1[C:5]2[C:6]3[C:11]([CH2:12][C:4]=2[C:3]([C:13]2[CH:18]=[CH:17][C:16]([OH:19])=[CH:15][CH:14]=2)=[N:2]1)=[CH:10][CH:9]=[CH:8][CH:7]=3.O[CH2:21][CH2:22][N:23]1[CH2:28][CH2:27][O:26][CH2:25][CH2:24]1.C1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1.CCOC(/N=N/C(OCC)=O)=O>ClCCl>[O:26]1[CH2:27][CH2:28][N:23]([CH2:22][CH2:21][O:19][C:16]2[CH:17]=[CH:18][C:13]([C:3]3[C:4]4[CH2:12][C:11]5[C:6](=[CH:7][CH:8]=[CH:9][CH:10]=5)[C:5]=4[NH:1][N:2]=3)=[CH:14][CH:15]=2)[CH2:24][CH2:25]1

참가 물질

6

반응물 4

HCID 11776TriphenylphosphineHCID 611632-MorpholinoethanolHCID 5462977Diethyl azodicarboxylateHCID 135512470HCID 135512470, 화합물

생성물 1

HCID 9906959HCID 9906959, 화합물

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

A mixture of 4-(1,4-dihydroindeno[1,2-c]pyrazol-3-yl)phenol (0.76 g, Example 30) 4-(2-hydroxyethyl)morpholine (0.85 g), triphenylphosphine (1.77 g) and dichloromethane (20 ml) were stirred together with ice/water bath cooling and diethylazodicarboxylate (1.16 g) was added dropwise. The resultant mixture was allowed to warm to room temperature and stirred for about 24 hours. The solvent was evaporated off under reduced pressure and the residue purified by flash column chromatography on silica using ethyl acetate/ethanol (25%) to give a solid. The solid was triturated with diethyl ether (10 ml) and the solid filtered, washed with diether and dried at about 65° C. to give 3-[4-(2-morpholinoethoxy)phenyl]-1,4-dihydroindeno[1,2-c]pyrazole, m.p. 175-6° C.

후처리

  1. temperaturecooling
  2. stirringstirred for about 24 hours
  3. customThe solvent was evaporated off under reduced pressure
  4. customthe residue purified by flash column chromatography on silica
  5. customto give a solid
  6. customThe solid was triturated with diethyl ether (10 ml)
  7. filtrationthe solid filtered
  8. washwashed with diether
  9. customdried at about 65° C.

출처 및 근거

ORD 기록
ord-224b351a3bf6493e84174d343b578f94
출처 데이터셋
uspto-grants-2002_10
특허 번호
US06462036B1

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