Triphenylphosphine → 2-(3,4,5-Tris(octadecyloxy)-cyclohexylmethoxy)-9-fluorenone

HRID 573035

反応式

HRID 573035 の反応式
[CH2:1]([O:19][CH:20]1[CH:25]([O:26][CH2:27][CH2:28][CH2:29][CH2:30][CH2:31][CH2:32][CH2:33][CH2:34][CH2:35][CH2:36][CH2:37][CH2:38][CH2:39][CH2:40][CH2:41][CH2:42][CH2:43][CH3:44])[CH:24]([O:45][CH2:46][CH2:47][CH2:48][CH2:49][CH2:50][CH2:51][CH2:52][CH2:53][CH2:54][CH2:55][CH2:56][CH2:57][CH2:58][CH2:59][CH2:60][CH2:61][CH2:62][CH3:63])[CH2:23][CH:22]([CH2:64][OH:65])[CH2:21]1)[CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][CH2:7][CH2:8][CH2:9][CH2:10][CH2:11][CH2:12][CH2:13][CH2:14][CH2:15][CH2:16][CH2:17][CH3:18].O[C:67]1[CH:79]=[CH:78][C:77]2[C:76]3[C:71](=[CH:72][CH:73]=[CH:74][CH:75]=3)[C:70](=[O:80])[C:69]=2[CH:68]=1.C1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1>C1COCC1>[CH2:1]([O:19][CH:20]1[CH:25]([O:26][CH2:27][CH2:28][CH2:29][CH2:30][CH2:31][CH2:32][CH2:33][CH2:34][CH2:35][CH2:36][CH2:37][CH2:38][CH2:39][CH2:40][CH2:41][CH2:42][CH2:43][CH3:44])[CH:24]([O:45][CH2:46][CH2:47][CH2:48][CH2:49][CH2:50][CH2:51][CH2:52][CH2:53][CH2:54][CH2:55][CH2:56][CH2:57][CH2:58][CH2:59][CH2:60][CH2:61][CH2:62][CH3:63])[CH2:23][CH:22]([CH2:64][O:65][C:67]2[CH:79]=[CH:78][C:77]3[C:76]4[C:71](=[CH:72][CH:73]=[CH:74][CH:75]=4)[C:70](=[O:80])[C:69]=3[CH:68]=2)[CH2:21]1)[CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][CH2:7][CH2:8][CH2:9][CH2:10][CH2:11][CH2:12][CH2:13][CH2:14][CH2:15][CH2:16][CH2:17][CH3:18]

参加物

5

反応物 3

HCID 11776TriphenylphosphineHCID 813862-Hydroxyfluoren-9-oneHCID 866457853,4,5-Tris(octadecyloxy)cyclohexylmethyl alcohol

生成物 1

HCID 594992172-(3,4,5-Tris(octadecyloxy)-cyclohexylmethoxy)-9-fluorenone収率 93%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

(3,4,5-Tris(octadecyloxy)-cyclohexyl)-methanol (82.5 mg, 89.7 μmol), 2-hydroxy-9-fluorenone (26.4 mg, 135 μmol) and triphenylphosphine (35.3 mg, 135 μmol) were dissolved in dehydrated THF (1.6 mL), DIED (27 μL, 137 μmol) was added, and the mixture was stirred for 1.5 hours. THF was evaporated, and 90% aqueous acetonitrile (10 mL) was added to the residue to allow crystallization. The crystals were filtered, and the obtained crystals were washed well with acetonitrile (10 mL) to give 2-(3,4,5-tris(octadecyloxy)-cyclohexylmethoxy)-9-fluorenone (91.2 mg, 83.1 μmol, 93%).

後処理

  1. additionDIED (27 μL, 137 μmol) was added
  2. customTHF was evaporated
  3. addition90% aqueous acetonitrile (10 mL) was added to the residue
  4. customcrystallization
  5. filtrationThe crystals were filtered
  6. washthe obtained crystals were washed well with acetonitrile (10 mL)

出典と根拠

ORDレコード
ord-6c43e07ebdcf4829b213a1b2d5287650
出典データセット
uspto-grants-2015_05
特許番号
US09029504B2

関連ノート

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