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Hydrochloric Acid → 4-(4-{3-[4-(2-Aminopropionyl)piperazin-1-yl]propoxy}phenyl)-tetrahydropyran-4-carbonitrile

HRID 272910
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HRID 272910 반응식
[N:1]1([CH2:7][CH2:8][CH2:9][O:10][C:11]2[CH:16]=[CH:15][C:14]([C:17]3([C:23]#[N:24])[CH2:22][CH2:21][O:20][CH2:19][CH2:18]3)=[CH:13][CH:12]=2)[CH2:6][CH2:5][NH:4][CH2:3][CH2:2]1.C1C=[CH:27][C:28]2[N:33](O)N=N[C:29]=2C=1.CCN=C=NCCCN(C)C.Cl.Cl.N1CCCCC1.[OH2:54]>C(Cl)Cl>[NH2:33][CH:28]([CH3:29])[C:27]([N:4]1[CH2:5][CH2:6][N:1]([CH2:7][CH2:8][CH2:9][O:10][C:11]2[CH:12]=[CH:13][C:14]([C:17]3([C:23]#[N:24])[CH2:22][CH2:21][O:20][CH2:19][CH2:18]3)=[CH:15][CH:16]=2)[CH2:2][CH2:3]1)=[O:54]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

8

반응물 6

HCID 313Hydrochloric AcidHCID 962Water2회HCID 8082PiperidineHCID 757711-HydroxybenzotriazoleHCID 27239391,3-Propanediamine, N'-(ethylcarbonimidoyl)-N,N-dimethyl-, monohydrochlorideHCID 598373994-[4-(3-Piperazin-1-ylpropoxy)phenyl]tetrahydropyran-4-carbonitrile

생성물 1

HCID 68577863
4-(4-{3-[4-(2-Aminopropionyl)piperazin-1-yl]propoxy}phenyl)-tetrahydropyran-4-carbonitrile
수율 42%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

4-[4-(3-piperazin-1-ylpropoxy)phenyl]tetrahydropyran-4-carbonitrile (265 mg, 0.81 mmol), DCM (10.6 ml), HOBT (120 mg, 0.89 mmol), FMoc (L)-aniline (277 mg, 0.89 mmol) and EDCl.HCl (171 mg, 0.89 mmol) were stirred at ambient temperature overnight. Water (10 ml) was added and stirred for one hour, the mixture was filtered and the organic phase separated and washed with water (10 ml), the organic phase was dried over MgSO4, filtered and concentrated in vacuo at 35° C. The residue was dissolved in DCM (9 ml) and piperidine (86 mg, 10 mmol) was added, the mixture was stirred at ambient temperature for one hour. To the reaction mixture, water (5 ml) was added and the organic phase separated, dried over MgSO4, filtered and concentrated in vacuo at 35° C. The crude material was subjected to chromatography on silica eluting with 2% MeOH in DCM to provide title compound (136 mg, 42%). 1H NMR (400 MHz, CDCl3), δ 7.38 (d, 2H), 6.93 (d, 2H), 4.11-4.05 (m, 2H), 4.03 (t, 2H), 3.89 (td, 2H), 3.77 (q, 1H), 3.65 (br s, 2H), 3.49 (br s, 2H), 2.55 (t, 2H), 2.45 (br s, 4H), 2.14-2.00 (m, 4H), 1.97 (m, 2H), 1.58 (br s, 2H), 1.25 (d, 3H).

후처리

  1. filtrationthe mixture was filtered
  2. customthe organic phase separated
  3. washwashed with water (10 ml)
  4. dry with materialthe organic phase was dried over MgSO4
  5. filtrationfiltered
  6. concentrationconcentrated in vacuo at 35° C
  7. dissolutionThe residue was dissolved in DCM (9 ml)
  8. stirringthe mixture was stirred at ambient temperature for one hour
  9. customthe organic phase separated
  10. dry with materialdried over MgSO4
  11. filtrationfiltered
  12. concentrationconcentrated in vacuo at 35° C

출처 및 근거

ORD 기록
ord-ad90d5eea6c84839a0d0132c8ea2e690
출처 데이터셋
uspto-grants-2008_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07456164B2

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