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Hydrogen Bromide → HCID 13711140, 화합물

HRID 280154
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HRID 280154 반응식
Br.C[O:3][C:4]1[CH:12]=[CH:11][CH:10]=[C:9]2[C:5]=1[CH2:6][CH2:7][CH:8]2[N:13]1[CH2:18][CH2:17][CH2:16][CH2:15][CH2:14]1.O.C>C(O)(=O)C.C(#N)C>[OH:3][C:4]1[CH:12]=[CH:11][CH:10]=[C:9]2[C:5]=1[CH2:6][CH2:7][CH:8]2[N:13]1[CH2:18][CH2:17][CH2:16][CH2:15][CH2:14]1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 4

HCID 260Hydrogen BromideHCID 297Methane2회HCID 962WaterHCID 13799019HCID 13799019, 화합물

생성물 1

HCID 13711140HCID 13711140, 화합물

시약·촉매·용매 2

HCID 176Acetic Acid용매HCID 6342
Acetonitrile
용매
2회

실험 절차

Hydrobromic acid (47-49%, 750 ml) is added to a stirred solution of the 4-methoxy-1-piperidinylindan (75 g) in glacial acetic acid (750 ml) under nitrogen. The mixture is refluxed for four hours, allowed to cool and poured into crushed ice and water. The pH of the ice mixture is adjusted to about 9 and the aqueous mixture extracted with methylene chloride. The methylene chloride extract is washed with water thereby forming a precipitate which is filtered and the solid dried. The methylene chloride layer is evaporated yielding an oil. The solid is dissolved in acetonitrile and treated with charcoal. The oil is treated with charcoal and dissolved in acetonitrile. Both dissolved materials are recrystallized from acetonitrile yielding the desired product, M.P. 134.5°-136.5° C.

후처리

  1. temperatureThe mixture is refluxed for four hours
  2. temperatureto cool
  3. additionpoured
  4. extractionthe aqueous mixture extracted with methylene chloride
  5. extractionThe methylene chloride extract
  6. washis washed with water
  7. customthereby forming a precipitate which
  8. filtrationis filtered
  9. customthe solid dried
  10. customThe methylene chloride layer is evaporated
  11. customyielding an oil
  12. customBoth dissolved materials are recrystallized from acetonitrile yielding the desired product, M.P. 134.5°-136.5° C.

출처 및 근거

ORD 기록
ord-b3c8baae30494e9989c22c9cea44b530
출처 데이터셋
uspto-grants-1986_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04588719

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