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Water → HCID 18783154, 화합물

HRID 1420879
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HRID 1420879 반응식
Cl.[CH3:2][C:3]1([NH2:13])[CH2:8][C:7]([CH3:10])([CH3:9])[CH2:6][C:5]([CH3:12])([CH3:11])[CH2:4]1.Br[CH2:15][CH2:16][CH2:17][C:18]#[N:19].C(=O)([O-])[O-].[Na+].[Na+].O>O1CCCC1>[C:18]([CH2:17][CH2:16][CH2:15][NH:13][C:3]1([CH3:2])[CH2:8][C:7]([CH3:10])([CH3:9])[CH2:6][C:5]([CH3:12])([CH3:11])[CH2:4]1)#[N:19]
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참가 물질

6

반응물 4

HCID 962WaterHCID 10340Sodium CarbonateHCID 214124-BromobutyronitrileHCID 98591051,3,3,5,5-pentamethylcyclohexan-1-amine Hydrochloride

생성물 1

HCID 18783154HCID 18783154, 화합물수율 86%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

A mixture of 1,3,3,5,5-pentamethylcyclohexylamine hydrochloride (1) (2-06 g, 10 mmol) 4-bromobutyronitrile (1.55 g. 10.5 mmol) and sodium carbonate (3.18 g, 30 mmol) in tetrahydrofuran (50 ml) was refluxed for 85 h, the poured into water (100 ml) and extracted with ether (3*30 ml). The combined organic phases were washed with brine (20 ml) and dried over K2CO3. The solution was filtered and evaporated and the crude product was purified by chromatography on silica gel, eluting with hexane-ether (10:1), (6:1), (4:1) to give product 2 (1.86 g, 86%) as an colorless oil.

후처리

  1. temperaturewas refluxed for 85 h
  2. extractionextracted with ether (3*30 ml)
  3. washThe combined organic phases were washed with brine (20 ml)
  4. dry with materialdried over K2CO3
  5. filtrationThe solution was filtered
  6. customevaporated
  7. customthe crude product was purified by chromatography on silica gel
  8. washeluting with hexane-ether (10:1), (6:1), (4:1)

출처 및 근거

ORD 기록
ord-a796cfcc63e2414485e2d642bfbfeadf
출처 데이터셋
uspto-grants-2000_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06071966

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