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Ammonia → HCID 22758136, 화합물

HRID 1287275
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HRID 1287275 반응식
[CH3:1][N:2]([CH3:15])[CH2:3][CH2:4][CH2:5][C:6]1[C:14]2[C:9](=[CH:10][CH:11]=[CH:12][CH:13]=2)[CH2:8][CH:7]=1.CCOCC.N.[Li]>C(O)C>[CH3:15][N:2]([CH3:1])[CH2:3][CH2:4][CH2:5][CH:6]1[C:14]2[CH2:13][CH:12]=[CH:11][CH2:10][C:9]=2[CH2:8][CH2:7]1
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HCID 222Ammonia2회HCID 3283Diethyl EtherHCID 3028194LithiumHCID 22758131N,N-Dimethylinden-3-propylamine

생성물 1

HCID 22758136HCID 22758136, 화합물

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

A solution of 35 g. (0.174 mole) of N,N-dimethylinden-3-propylamine in a total volume of 125 ml. of ether is added to 2 liters of liquid ammonia. Over 1 hr., 44 g. (6.3 g-atoms) of lithium ribbon is added at the reflux temperature. After a total of 3 hours, the reaction mixture is blue. 550 ml. of ethanol is added over 135 min. whereupon the blue color fades. The ammonia is allowed to evaporate overnight and the residue dissolved in 1500 ml. of water and extracted twice with ether. The ether extract gives 34.5 g. (98.6%) of crude diene upon drying and solvent removal which contains ca, 10% of the corresponding aromatic compound by nmr integration.

후처리

  1. customAfter a total of 3 hours
  2. customto evaporate overnight
  3. dissolutionthe residue dissolved in 1500 ml
  4. extractionof water and extracted twice with ether
  5. extractionThe ether extract
  6. customgives 34.5 g
  7. dry with material(98.6%) of crude diene upon drying
  8. customsolvent removal which

출처 및 근거

ORD 기록
ord-708f758ae3b747f1b8d6dccd8a0aa514
출처 데이터셋
uspto-grants-1976_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US03984407

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