Tetrahydrofuran → HCID 18402528、化合物

HRID 1018801

反応式

HRID 1018801 の反応式
C([Li])CCC.Br[C:7]1[CH:12]=[CH:11][C:10]([C:13]([O:17][CH3:18])([O:15][CH3:16])[CH3:14])=[CH:9][CH:8]=1.[CH3:19][C:20]1([CH3:26])[CH2:25][CH2:24][CH2:23][CH2:22][CH2:21]1.[O:27]1CCCC1>C1CCCCC1>[CH3:16][O:15][C:13]([C:10]1[CH:11]=[CH:12][C:7]([C:23]2([OH:27])[CH2:24][CH2:25][C:20]([CH3:26])([CH3:19])[CH2:21][CH2:22]2)=[CH:8][CH:9]=1)([O:17][CH3:18])[CH3:14]

参加物

6

反応物 4

HCID 8028Tetrahydrofuran2 回HCID 115491,1-DimethylcyclohexaneHCID 109117821-Bromo-4-(1,1-dimethoxyethyl)benzeneHCID 178418339Butyllithium

生成物 1

HCID 18402528HCID 18402528、化合物

試薬・触媒・溶媒 1

HCID 8078Cyclohexane溶媒

反応条件

温度
-78 °C

実験手順

328 ml of a 1.6 M solution of butyllithium in cyclohexane are added at −78° C. to 117 g of 1-bromo-4-(1,1-dimethoxyethyl)benzene in 1100 ml of tetrahydrofuran and the reaction mixture is stirred at −78° C. for 2 hours. 66 g of 4,4-dimethylcyclohexane dissolved in 210 ml of tetrahydrofuran are added at this same temperature and the reaction mixture is stirred for 1 hour at −78° C. The reaction mixture is hydrolysed by addition of crushed ice. The organic phase is separated out after settling of the phases has taken place, it is dried over sodium sulphate and the solvents are evaporated off under reduced pressure. The compound obtained is recrystallized from 500 ml of n-hexane; m.p.=88° C.

後処理

  1. additionare added at this same temperature
  2. stirringthe reaction mixture is stirred for 1 hour at −78° C
  3. additionThe reaction mixture is hydrolysed by addition of crushed ice
  4. customThe organic phase is separated out
  5. dry with materialis dried over sodium sulphate
  6. customthe solvents are evaporated off under reduced pressure
  7. customThe compound obtained
  8. customis recrystallized from 500 ml of n-hexane

出典と根拠

ORDレコード
ord-44b86795716e4ad79350c88828f2e8e9
出典データセット
uspto-grants-2002_11
特許番号
US06482986B1

関連ノート

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