Water → HCID 68800602, 화합물

HRID 1434496노트

반응식

HRID 1434496 반응식
[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]

참가 물질

5

반응물 3

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

생성물 1

HCID 68800602HCID 68800602, 화합물

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

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).

후처리

  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)

출처 및 근거

ORD 기록
ord-990f80f0a1134d03a4f209e688249faa
출처 데이터셋
uspto-grants-2009_11
특허 번호
US07615289B2

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