Water → HCID 68800602、化合物

HRID 1434496ノート

反応式

HRID 1434496 の反応式
[CH2:1]([C:7]1([CH2:21][CH2:22][CH2:23][CH2:24][CH2:25][CH3:26])[C:19]2[CH:18]=[C:17](Br)[CH:16]=[CH:15][C:14]=2[C:13]2[C:8]1=[CH:9][CH:10]=[CH:11][CH:12]=2)[CH2:2][CH2:3][CH2:4][CH2:5][CH3:6].[Br:27][C:28]1[C:29](=O)[C:30]2[C:38](=[CH:39][CH:40]=1)[C:37]1[C:32](=[CH:33][C:34]([Br:41])=[CH:35][CH:36]=1)[CH:31]=2.[OH2:43]>C1COCC1>[CH2:21]([C:7]1([CH2:1][CH2:2][CH2:3][CH2:4][CH2:5][CH3:6])[C:19]2[CH:18]=[C:17]([C:31]3([OH:43])[C:30]4[CH:29]=[C:28]([Br:27])[CH:40]=[CH:39][C:38]=4[C:37]4[C:32]3=[CH:33][C:34]([Br:41])=[CH:35][CH:36]=4)[CH:16]=[CH:15][C:14]=2[C:13]2[C:8]1=[CH:9][CH:10]=[CH:11][CH:12]=2)[CH2:22][CH2:23][CH2:24][CH2:25][CH3:26]

参加物

5

反応物 3

HCID 962WaterHCID 186746002-Bromo-9,9-dihexyl fluoreneHCID 534201032,7Dibromofluorenone

生成物 1

HCID 68800602HCID 68800602、化合物

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

To 5.64 g of Mg placed into a 1000 ml three-neck flask, 80 g of 9,9-dihexyl-2-bromofluorene in 300 ml THF was slowly added dropwise, to prepare a Grignard reagent. After a temperature of a reaction chamber was decreased to −40° C. or less, 52 g of 2,7-dibromofluorenone was added to the reaction bath in a nitrogen atmosphere. The temperature was gradually increased to room temperature, followed by stirring for 10 hours. The resulting reaction solution was poured into water, after which an extraction was performed using diethyl ether. The solvent was evaporated using a rotary evaporator. A column chromatography separation resulted in 60 g (58%) of (9-(9,9-dihexylfluoren-2-yl)-2,7-dibromofluoren-9-ol) (1).

後処理

  1. customwas decreased to −40° C. or less
  2. customThe resulting reaction solution
  3. extractionafter which an extraction
  4. customThe solvent was evaporated
  5. customa rotary evaporator
  6. customA column chromatography separation
  7. customresulted in 60 g (58%) of (9-(9,9-dihexylfluoren-2-yl)-2,7-dibromofluoren-9-ol) (1)

出典と根拠

ORDレコード
ord-990f80f0a1134d03a4f209e688249faa
出典データセット
uspto-grants-2009_11
特許番号
US07615289B2

反応ノート

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