Tetrahydrofuran → 9,9-dibutyl-2-iodo-9H-fluorene

HRID 221174

반응식

HRID 221174 반응식
[I:1][C:2]1[CH:14]=[CH:13][C:12]2[C:11]3[C:6](=[CH:7][CH:8]=[CH:9][CH:10]=3)[CH2:5][C:4]=2[CH:3]=1.I[CH2:16][CH2:17][CH2:18][CH3:19].CC(C)([O-])C.[K+].O1[CH2:30][CH2:29][CH2:28][CH2:27]1>C(OCC)C.O>[CH2:16]([C:5]1([CH2:27][CH2:28][CH2:29][CH3:30])[C:4]2[CH:3]=[C:2]([I:1])[CH:14]=[CH:13][C:12]=2[C:11]2[C:6]1=[CH:7][CH:8]=[CH:9][CH:10]=2)[CH2:17][CH2:18][CH3:19]

참가 물질

7

반응물 4

HCID 8028TetrahydrofuranHCID 10962Butyl iodideHCID 2240942-Iodo-9H-fluoreneHCID 23665647Potassium tert-butoxide

생성물 1

HCID 230728539,9-dibutyl-2-iodo-9H-fluorene

시약·촉매·용매 2

HCID 962Water용매HCID 3283Diethyl Ether용매

반응 조건

온도
50 °C

실험 절차

Under N2 atmosphere, 0.58 parts of 2-iodo-9H-fluorene, 1.10 parts of 1-iodobutane, and 0.67 parts of potassium tert-butoxide were added into 15 parts of dry tetrahydrofuran, followed by stirring and mixing. Then, the reaction mixture was heated to 50° C. and reacted for 12 hours. After the reaction mixture was cooled, poured the water into the reaction mixture for quenching the reaction, using the diethyl ether to extract the product, and magnesium sulfate was used for dehydration. After removing the solvent, the residual was purified with column chromatography method by using hexane as an eluent, to obtain a compound (32) of the present example. This compound was in a form of a light yellow solid, and the yield of this compound was 94%.

후처리

  1. additionmixing
  2. customreacted for 12 hours
  3. temperatureAfter the reaction mixture was cooled
  4. customfor quenching
  5. customthe reaction
  6. extractionto extract the product, and magnesium sulfate
  7. customAfter removing the solvent
  8. customthe residual was purified with column chromatography method

출처 및 근거

ORD 기록
ord-67fe20fafb014f069195b70da1c871fe
출처 데이터셋
uspto-grants-2012_06
특허 번호
US08203068B2

연결된 노트

불러오는 중…