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Hydrogen Bromide → HCID 68144948, 화합물

HRID 1576667
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HRID 1576667 반응식
[OH:1][C:2]1([C:8]2[CH:13]=[CH:12][C:11]3[O:14][CH2:15][O:16][C:10]=3[CH:9]=2)[CH2:7][CH2:6][NH:5][CH2:4][CH2:3]1.[CH2:17](Br)[CH:18]=[CH:19][C:20]1[CH:25]=[CH:24][CH:23]=[CH:22][CH:21]=1.Br.N1(O)CCCCC1>CC(C)=O>[CH2:17]([N:5]1[CH2:6][CH2:7][C:2]([OH:1])([C:8]2[CH:13]=[CH:12][C:11]3[O:14][CH2:15][O:16][C:10]=3[CH:9]=2)[CH2:3][CH2:4]1)[CH:18]=[CH:19][C:20]1[CH:25]=[CH:24][CH:23]=[CH:22][CH:21]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 260Hydrogen BromideHCID 209351-HydroxypiperidineHCID 98116BromomethylstyreneHCID 150347154-(1,3-Benzodioxol-5-yl)piperidin-4-ol

생성물 1

HCID 68144948HCID 68144948, 화합물

시약·촉매·용매 1

HCID 180Acetone용매

실험 절차

4.4 g. 4-hydroxy-4-(3.4-methylene dioxy phenyl) -piperidine are dissolved hot in 75 ml. acetone, the solution obtained is mixed with 2.5 g. cinnamyl bromide and the reaction mixture is heated at reflux to boiling over the course of 4 hours. After boiling for 1 hour, part of the hydrobromide of the piperidinol used as the starting compound forms a precipitate and this is filtered off on completion of the reaction. The filtrate is then evaporated to dryness and extracted 3 times with 70 ml. ether each time. The ether solutions are combined, concentrated and mixed with petroleum ether during which time 1-cinnamyl-4-hydroxy-4-(3.4-methylene dioxy phenyl)-piperidine with a melting point of 114° - 115°C precipitates.

후처리

  1. additionis mixed with 2.5 g
  2. temperatureat reflux
  3. customto boiling over the course of 4 hours
  4. filtrationthis is filtered off on completion of the reaction
  5. customThe filtrate is then evaporated to dryness
  6. extractionextracted 3 times with 70 ml
  7. concentrationconcentrated
  8. additionmixed with petroleum ether during which time 1-cinnamyl-4-hydroxy-4-(3.4-methylene dioxy phenyl)-piperidine with a melting point of 114° - 115°C
  9. customprecipitates

출처 및 근거

ORD 기록
ord-f57d9905aa174052ad51d68cc7b89f75
출처 데이터셋
uspto-grants-1976_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US03982001

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