Triphenylphosphine → HCID 9906959、化合物

HRID 991015ノート

反応式

HRID 991015 の反応式
[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

参加物

6

反応物 4

HCID 11776TriphenylphosphineHCID 611632-MorpholinoethanolHCID 5462977Diethyl azodicarboxylateHCID 135512470HCID 135512470、化合物

生成物 1

HCID 9906959HCID 9906959、化合物

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

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.

後処理

  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.

出典と根拠

ORDレコード
ord-224b351a3bf6493e84174d343b578f94
出典データセット
uspto-grants-2002_10
特許番号
US06462036B1

反応ノート

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