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

HRID 221174

反応式

HRID 221174 の反応式
[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]

参加物

7

反応物 4

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

生成物 1

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

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 3283Diethyl Ether溶媒

反応条件

温度
50 °C

実験手順

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%.

後処理

  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

出典と根拠

ORDレコード
ord-67fe20fafb014f069195b70da1c871fe
出典データセット
uspto-grants-2012_06
特許番号
US08203068B2

関連ノート

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