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Hydrochloric Acid → 1-[2-Chloro-4-(2-diethylaminoethoxy)phenyl]-2-methylene-1-butanone

HRID 66604
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HRID 66604 반응식
[Cl:1][C:2]1[CH:7]=[C:6]([O:8][CH2:9][CH2:10][N:11]([CH2:14][CH3:15])[CH2:12][CH3:13])[CH:5]=[CH:4][C:3]=1[C:16](=[O:20])[CH2:17][CH2:18][CH3:19].Cl.[CH3:22]NC.C=O.Cl>>[Cl:1][C:2]1[CH:7]=[C:6]([O:8][CH2:9][CH2:10][N:11]([CH2:12][CH3:13])[CH2:14][CH3:15])[CH:5]=[CH:4][C:3]=1[C:16](=[O:20])[C:17](=[CH2:22])[CH2:18][CH3:19]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 4

HCID 313Hydrochloric AcidHCID 712FormaldehydeHCID 10473Dimethylamine, hydrochlorideHCID 130523711-[2-Chloro-4-(2-diethylaminoethoxy)phenyl]-1-butanone

생성물 1

HCID 130523721-[2-Chloro-4-(2-diethylaminoethoxy)phenyl]-2-methylene-1-butanone

실험 절차

A mixture of 8.9 g. (0.03 mole) of 1-[2-chloro-4-(2-diethylaminoethoxy)phenyl]-1-butanone, 2.7 g. (0.033 mole) of dimethylamine hydrochloride, 1.8 g. (0.06 mole) of paraformaldehyde and 5 ml. of concentrated hydrochloric acid is heated on the steam bath for 2 hours. The mixture is digested on the steam bath with 700 ml. of water, filtered and the filtrate added to 350 ml. of 10% aqueous sodium bicarbonate. The solution is heated on the steam bath for 1 hr., cooled and extracted with ether. The ether extract is washed with water, dried over sodium sulfate, filtered and evaporated to dryness on the steam bath. The product is obtained upon distillation in vacuo (0.3 mm.) as a pale yellow oil.

후처리

  1. additionA mixture of 8.9 g
  2. filtrationof water, filtered
  3. additionthe filtrate added to 350 ml
  4. temperatureThe solution is heated on the steam bath for 1 hr
  5. temperature, cooled
  6. extractionextracted with ether
  7. extractionThe ether extract
  8. washis washed with water
  9. dry with materialdried over sodium sulfate
  10. filtrationfiltered
  11. customevaporated to dryness on the steam bath
  12. customThe product is obtained upon distillation in vacuo (0.3 mm.) as a pale yellow oil

출처 및 근거

ORD 기록
ord-f09433f7adb14145a79980c356699f18
출처 데이터셋
uspto-grants-1982_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04342782

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