Tetrahydrofuran → HCID 18402528, 화합물

HRID 1018801

반응식

HRID 1018801 반응식
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]

참가 물질

6

반응물 4

HCID 8028Tetrahydrofuran2회HCID 115491,1-DimethylcyclohexaneHCID 109117821-Bromo-4-(1,1-dimethoxyethyl)benzeneHCID 178418339Butyllithium

생성물 1

HCID 18402528HCID 18402528, 화합물

시약·촉매·용매 1

HCID 8078Cyclohexane용매

반응 조건

온도
-78 °C

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-44b86795716e4ad79350c88828f2e8e9
출처 데이터셋
uspto-grants-2002_11
특허 번호
US06482986B1

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