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Potassium Hydroxide → 2,3,4,5-tetrahydro-8-(phenyl-methoxy)-5-(phenylmethyl)-1H-pyrido[4,3-b]indole

HRID 1634182
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HRID 1634182 반응식
[C:1]1([CH2:7][O:8][C:9]2[CH:17]=[CH:16][C:15]3[N:14]([CH2:18][C:19]4[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=4)[C:13]4[CH2:25][CH2:26][N:27](C(OCC)=O)[CH2:28][C:12]=4[C:11]=3[CH:10]=2)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.[OH-].[K+]>CC(O)C>[C:1]1([CH2:7][O:8][C:9]2[CH:17]=[CH:16][C:15]3[N:14]([CH2:18][C:19]4[CH:20]=[CH:21][CH:22]=[CH:23][CH:24]=4)[C:13]4[CH2:25][CH2:26][NH:27][CH2:28][C:12]=4[C:11]=3[CH:10]=2)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 14797Potassium HydroxideHCID 18677421ethyl 1,3,4,5-tetrahydro-8-(phenyl-methoxy)-5-(phenyl-methyl)-2H-pyrido[4,3-b]indole-2-carboxylate

생성물 1

HCID 186774152,3,4,5-tetrahydro-8-(phenyl-methoxy)-5-(phenylmethyl)-1H-pyrido[4,3-b]indole수율 92%

시약·촉매·용매 1

HCID 3776Isopropanol용매

실험 절차

A mixture of intermediate (2) (0.067 mol) and KOH (0.67 mol) in 2-propanol (250 ml) was stirred and refluxed for 5 hours. The solvent was evaporated. Water (300 ml) was added and the organic solvent was removed azeotropically. The precipitate was filtered off and dissolved in CH2Cl2 (300 ml). The organic solution was dried, filtered and the solvent was evaporated. The residue was washed in CH3CN (50 ml), filtered off and dried, yielding 22.7 g (92%) of 2,3,4,5-tetrahydro-8-(phenylmethoxy)-5-(phenylmethyl)-1H-pyrido[4,3-b]indole (intermediate 3).

후처리

  1. temperaturerefluxed for 5 hours
  2. customThe solvent was evaporated
  3. additionWater (300 ml) was added
  4. customthe organic solvent was removed azeotropically
  5. filtrationThe precipitate was filtered off
  6. dissolutiondissolved in CH2Cl2 (300 ml)
  7. customThe organic solution was dried
  8. filtrationfiltered
  9. customthe solvent was evaporated
  10. washThe residue was washed in CH3CN (50 ml)
  11. filtrationfiltered off
  12. customdried

출처 및 근거

ORD 기록
ord-3bdcf4cc03204ea0b5f15189e6cbc91b
출처 데이터셋
uspto-grants-2003_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06506768B2

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