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Hydrochloric Acid → Hydrochloric Acid

HRID 875965
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HRID 875965 반응식
[Cl:1][C:2]1[C:7]2[N:8]([CH:35]3[CH2:39][CH2:38][CH2:37][CH2:36]3)[C:9]3[N:10]=[C:11]([NH:15][C:16]4[N:21]=[CH:20][C:19]([N:22]5[CH2:27][CH2:26][N:25](C(OC(C)(C)C)=O)[CH2:24][CH2:23]5)=[CH:18][CH:17]=4)[N:12]=[CH:13][C:14]=3[C:6]=2[CH:5]=[CH:4][N:3]=1.[ClH:40].O1CCOCC1>C(Cl)Cl.CCOCC>[Cl:1][C:2]1[C:7]2[N:8]([CH:35]3[CH2:39][CH2:38][CH2:37][CH2:36]3)[C:9]3[N:10]=[C:11]([NH:15][C:16]4[CH:17]=[CH:18][C:19]([N:22]5[CH2:23][CH2:24][NH:25][CH2:26][CH2:27]5)=[CH:20][N:21]=4)[N:12]=[CH:13][C:14]=3[C:6]=2[CH:5]=[CH:4][N:3]=1.[ClH:40]
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참가 물질

7

반응물 3

HCID 313Hydrochloric AcidHCID 312751,4-DioxaneHCID 58299799tert-Butyl 4-(6-((8-chloro-9-cyclopentyl-9H-pyrido[4',3':4,5]pyrrolo[2,3-d]-pyrimidin-2-yl)amino)-3-pyridinyl)-1-piperazinecarboxylate

생성물 2

HCID 313Hydrochloric Acid수율 100%HCID 58299601HCID 58299601, 화합물

시약·촉매·용매 2

HCID 3283
Diethyl Ether
용매
HCID 6344Dichloromethane용매

실험 절차

Compound 197 (0.173 g, 0.315 mmol) was dissolved in 10 mL of DCM and to this was added 4N HCl in dioxane (1.97 mL, 7.88 mmol). The solution was stirred at room temperature overnight and then concentrated under vacuum to give a yellow solid. The solid obtained was sonicated in Et2O and a yellowish solid was collected on filter paper to give compound 190 as an HCl salt (0.164 g, 100%). 1H NMR (500 MHz, DMSO-d6) δ 10.56 (1 H, br. s.), 9.42 (1 H, s), 8.87 (2 H, br. s.), 8.28 (1 H, d, J=4.9 Hz), 8.19 (1 H, d, J=5.1 Hz), 8.09 (1 H, d, J=2.9 Hz), 7.97 (1 H, d, J=9.0 Hz), 7.75 (1 H, dd, J=9.3, 2.0 Hz), 5.96-6.07 (2 H, m, J=9.2, 8.9, 8.8, 8.8 Hz), 3.37-3.43 (4 H, m), 3.26-3.33 (4 H, m), 2.54-2.65 (2 H, m), 2.01-2.12 (4 H, m), 1.66-1.77 (2 H, m) ppm; LCMS-ESI (POS), M/Z, M+1: Found 449.2.

후처리

  1. concentrationconcentrated under vacuum
  2. customto give a yellow solid
  3. customThe solid obtained
  4. customa yellowish solid was collected
  5. filtrationon filter paper

출처 및 근거

ORD 기록
ord-5a92201649c549f699feacbed2e9fb68
출처 데이터셋
uspto-grants-2015_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08980903B2

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