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1,3-Dibromobutane → HCID 22995747, 화합물

HRID 1167110
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HRID 1167110 반응식
C([Li])CCC.C(NC(C)C)(C)C.[C:13]1([CH:19]([CH2:25][CH3:26])[CH2:20][C:21]([O:23][CH3:24])=[O:22])[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=1.[Br:27][CH2:28][CH2:29][CH:30](Br)[CH3:31]>CCCCCC.O1CCCC1>[Br:27][CH2:28][CH2:29][CH2:30][CH2:31][C:19]([CH2:25][CH3:26])([C:13]1[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=1)[CH2:20][C:21]([O:23][CH3:24])=[O:22]
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 4

HCID 78891,3-DibromobutaneHCID 7912DiisopropylamineHCID 578303HCID 578303, 화합물HCID 178418339Butyllithium

생성물 1

HCID 22995747HCID 22995747, 화합물

시약·촉매·용매 2

HCID 8028Tetrahydrofuran용매
HCID 8058
Hexane
용매

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온도
-10 °C

실험 절차

40 ml (0.1 mol) of n-butyl lithium as a 2.5 molar solution in hexane are added dropwise to a solution of 14 ml (0.1 mol) of diisopropylamine in 150 ml of anhydrous tetrahydrofuran at −30° C. and stirred for 10 minutes at −10° C. At −76° C., 16.4 g (0.1 mol) of methyl 2-phenylbutanecarboxylate are added dropwise and the mixture is stirred for 30 minutes at this temperature. Then 12.12 ml (0.101 mol) of 1,3-dibromobutane are added, when the addition has ended the cooling bath is removed and the mixture is stirred for 14 hours at ambient temperature. The reaction solution is poured onto 1.2 l water and extracted with diethylether. The organic phases are extracted with water, dried over sodium sulphate and the solvent is eliminated. The residue is distilled under high vacuum.

후처리

  1. stirringthe mixture is stirred for 30 minutes at this temperature
  2. additionwhen the addition
  3. customis removed
  4. stirringthe mixture is stirred for 14 hours at ambient temperature
  5. additionThe reaction solution is poured onto 1.2 l water
  6. extractionextracted with diethylether
  7. extractionThe organic phases are extracted with water
  8. dry with materialdried over sodium sulphate
  9. distillationThe residue is distilled under high vacuum

출처 및 근거

ORD 기록
ord-326b983a529647d2bbbdd1720fd3266e
출처 데이터셋
uspto-grants-2003_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06617325B1

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