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Hydrochloric Acid → 1,2,3,3a,4,8b-Hexahydrocyclopenta[b]indole

HRID 916621
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HRID 916621 반응식
[CH2:1]1[C:12]2[C:11]3[CH:10]=[CH:9][CH:8]=[CH:7][C:6]=3[NH:5][C:4]=2[CH2:3][CH2:2]1.Cl>[Pd]>[CH2:1]1[CH:12]2[CH:4]([NH:5][C:6]3[CH:7]=[CH:8][CH:9]=[CH:10][C:11]=32)[CH2:3][CH2:2]1
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참가 물질

4

반응물 2

HCID 313Hydrochloric AcidHCID 2703051,2,3,4-Tetrahydro-cyclopenta(b)indole

생성물 1

HCID 218735741,2,3,3a,4,8b-Hexahydrocyclopenta[b]indole수율 69.1%

시약·촉매·용매 1

HCID 23938Palladium촉매

실험 절차

A mixture of 1,2,3,4-tetrahydrocyclopenta[b]indole (11 mmol, 1.8 g), 5% Pd/C (0.5 g), and concentrated hydrochloric acid (1.2 mL) was hydrogenated at 45 psi on a Parr shaker. After 3 h, the mixture was removed from the shaker and filtered through Celite. The solid bed was washed with methanol. The filtrate was concentrated. The crude oil was dissolved in 1 N HCl and washed with ether. The aqueous phase was treated with 2.5 N NaOH to pH>10 and then extracted with chloroform. The combined chloroform extracts were dried over MgSO4, filtered and concentrated to give the crude indoline. The material was purified by flash column chromatography through silica gel (Biotage, elution with 10% ethyl acetate-hexanes) to give the known indoline (7.6 mmol, 1.2 g, 69%) as a clear oil.

후처리

  1. customthe mixture was removed from the shaker
  2. filtrationfiltered through Celite
  3. washThe solid bed was washed with methanol
  4. concentrationThe filtrate was concentrated
  5. dissolutionThe crude oil was dissolved in 1 N HCl
  6. washwashed with ether
  7. additionThe aqueous phase was treated with 2.5 N NaOH to pH>10
  8. extractionextracted with chloroform
  9. dry with materialThe combined chloroform extracts were dried over MgSO4
  10. filtrationfiltered
  11. concentrationconcentrated
  12. customto give the crude indoline
  13. customThe material was purified by flash column chromatography through silica gel (Biotage, elution with 10% ethyl acetate-hexanes)

출처 및 근거

ORD 기록
ord-9465440f448d42d092d761c1007da0d4
출처 데이터셋
uspto-grants-2007_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07271163B2

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