Potassium Carbonate → 4-[2-(9,9-Dibutyl-7-ethynyl-9H-fluoren-2-yl)ethynyl]-N,N-dihexylbenzenamine

HRID 41811

반응식

HRID 41811 반응식
C([O-])([O-])=O.[K+].[K+].[CH2:7]([C:11]1([CH2:51][CH2:52][CH2:53][CH3:54])[C:23]2[CH:22]=[C:21]([CH2:24][C:25](C)(O)C#C)[CH:20]=[CH:19][C:18]=2[C:17]2[C:12]1=[CH:13][C:14]([C:30]#[C:31][C:32]1[CH:37]=[CH:36][C:35]([N:38]([CH2:45][CH2:46][CH2:47][CH2:48][CH2:49][CH3:50])[CH2:39][CH2:40][CH2:41][CH2:42][CH2:43][CH3:44])=[CH:34][CH:33]=1)=[CH:15][CH:16]=2)[CH2:8][CH2:9][CH3:10]>C1(C)C=CC=CC=1.CC(O)C>[CH2:51]([C:11]1([CH2:7][CH2:8][CH2:9][CH3:10])[C:12]2[CH:13]=[C:14]([C:30]#[C:31][C:32]3[CH:33]=[CH:34][C:35]([N:38]([CH2:39][CH2:40][CH2:41][CH2:42][CH2:43][CH3:44])[CH2:45][CH2:46][CH2:47][CH2:48][CH2:49][CH3:50])=[CH:36][CH:37]=3)[CH:15]=[CH:16][C:17]=2[C:18]2[C:23]1=[CH:22][C:21]([C:24]#[CH:25])=[CH:20][CH:19]=2)[CH2:52][CH2:53][CH3:54]

참가 물질

4

반응물 2

HCID 11430Potassium CarbonateHCID 86646643[9,9-Dibutyl-7-[2-[4-(dihexylamino)phenyl]ethynyl]-9H-fluorene-2-yl]-2-methyl-3-butyn-2-ol

생성물 1

HCID 866466424-[2-(9,9-Dibutyl-7-ethynyl-9H-fluoren-2-yl)ethynyl]-N,N-dihexylbenzenamine수율 87%

시약·촉매·용매 1

HCID 21881414Toluene isopropyl alcohol용매

실험 절차

Potash powder (0.07 g) is added to a solution of 5a (0.798 g, 1.24 mmol) in 8.75 mL of toluene/i-PrOH (6/1). The mixture is heated in a reverse-flow boiler for 1 h. After cooling, the potash is filtered and the solvents are evaporated. The raw product is purified by silica gel column chromatography (heptane/CH2Cl2 90:10) to yield 0.632 g (87%) of 5b.

후처리

  1. temperatureThe mixture is heated in a reverse-flow boiler for 1 h
  2. temperatureAfter cooling
  3. filtrationthe potash is filtered
  4. customthe solvents are evaporated
  5. customThe raw product is purified by silica gel column chromatography (heptane/CH2Cl2 90:10)

출처 및 근거

ORD 기록
ord-03ed10cb8a41497eab0f16a59da04230
출처 데이터셋
uspto-grants-2013_09
특허 번호
US08535643B2

연결된 노트

불러오는 중…