Hydrochloric Acid → HCID 20031347, 화합물

HRID 232303노트

반응식

HRID 232303 반응식
Br[C:2]1[CH:7]=[CH:6][C:5]([F:8])=[CH:4][CH:3]=1.[Mg].[CH2:10]([N:14]1[CH2:20][CH2:19][CH2:18][CH2:17][CH:16]([C:21]#N)[CH2:15]1)[CH2:11][CH2:12][CH3:13].Cl.CC[O:26]CC>>[F:8][C:5]1[CH:6]=[CH:7][C:2]([C:21]([CH:16]2[CH2:17][CH2:18][CH2:19][CH2:20][N:14]([CH2:10][CH2:11][CH2:12][CH3:13])[CH2:15]2)=[O:26])=[CH:3][CH:4]=1

참가 물질

6

반응물 5

HCID 313Hydrochloric AcidHCID 3283Diethyl EtherHCID 99931-Bromo-4-fluorobenzeneHCID 5462224Magnesium2회HCID 20031349HCID 20031349, 화합물

생성물 1

HCID 20031347HCID 20031347, 화합물

실험 절차

To 25 mL of dry ether under N2 add 2 g (11 mmol) of 1-bromo-4-fluorobenzene and 0.25 g (0.10 mmol) of magnesium turnings. Initiate the reaction by standard procedures. When the magnesium filings are gone add 1 g (8.0 mmol) of 1-butyl-hexahydro-1H-azepine-3-carbonitrile and reflux the reaction mixture. Monitor the reaction by thin-layer chromatography. Upon completion add 50 mL 1M HCl and stir for one hr. The layers are separated and the aqueous layer is extracted with methylene chloride (25 mL). Add 4N NaOH to the aqueous layer until basic and extract with methylene chloride. Dry the organic phase over Na2SO4. Filter off the drying agent and evaporate the solvent in vacuo to obtain the title compound.

후처리

  1. customInitiate the reaction by standard procedures
  2. temperaturereflux the reaction mixture
  3. customMonitor the reaction by thin-layer chromatography
  4. customThe layers are separated
  5. extractionthe aqueous layer is extracted with methylene chloride (25 mL)
  6. additionAdd 4N NaOH to the aqueous layer until basic and
  7. extractionextract with methylene chloride
  8. dry with materialDry the organic phase over Na2SO4
  9. filtrationFilter off the drying agent
  10. customevaporate the solvent in vacuo

출처 및 근거

ORD 기록
ord-ed65bd1748e74875b5be36b0d3ec3e25
출처 데이터셋
uspto-grants-1989_07
특허 번호
US04851526

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