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Hydrochloric Acid → 5-{1-[(2,5-difluorophenyl)acetyl]-2,3-dihydro-1H-indol-5-yl}-7-[2-(4-piperidinyl)ethyl]-7H-pyrrolo[2,3-d]pyrimidin-4-amine

HRID 1910058
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HRID 1910058 반응식
[NH2:1][C:2]1[C:3]2[C:10]([C:11]3[CH:12]=[C:13]4[C:17](=[CH:18][CH:19]=3)[N:16]([C:20](=[O:30])[CH2:21][C:22]3[CH:27]=[C:26]([F:28])[CH:25]=[CH:24][C:23]=3[F:29])[CH2:15][CH2:14]4)=[CH:9][N:8]([CH2:31][CH2:32][CH:33]3[CH2:38][CH2:37][N:36](C(OC(C)(C)C)=O)[CH2:35][CH2:34]3)[C:4]=2[N:5]=[CH:6][N:7]=1.Cl>O1CCOCC1>[F:29][C:23]1[CH:24]=[CH:25][C:26]([F:28])=[CH:27][C:22]=1[CH2:21][C:20]([N:16]1[C:17]2[C:13](=[CH:12][C:11]([C:10]3[C:3]4[C:2]([NH2:1])=[N:7][CH:6]=[N:5][C:4]=4[N:8]([CH2:31][CH2:32][CH:33]4[CH2:34][CH2:35][NH:36][CH2:37][CH2:38]4)[CH:9]=3)=[CH:19][CH:18]=2)[CH2:14][CH2:15]1)=[O:30]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 313Hydrochloric AcidHCID 668239521,1-dimethylethyl 4-[2-(4-amino-5-{1-[(2,5-difluorophenyl)acetyl]-2,3-dihydro-1H-indol-5-yl}-7H-pyrrolo[2,3-d]pyrimidin-7-yl)ethyl]-1-piperidinecarboxylate

생성물 1

HCID 668236715-{1-[(2,5-difluorophenyl)acetyl]-2,3-dihydro-1H-indol-5-yl}-7-[2-(4-piperidinyl)ethyl]-7H-pyrrolo[2,3-d]pyrimidin-4-amine수율 87.3%

시약·촉매·용매 1

HCID 312751,4-Dioxane용매

실험 절차

To 1,1-dimethylethyl 4-[2-(4-amino-5-{1-[(2,5-difluorophenyl)acetyl]-2,3-dihydro-1H-indol-5-yl}-7H-pyrrolo[2,3-d]pyrimidin-7-yl)ethyl]-1-piperidinecarboxylate (157 mg, 0.255 mmol) was added 4N HCl (5 mL, 20.00 mmol) in dioxane and the mixture was allowed to stir at room temperature overnight. The reaction was concentrated and the solid was isolated by filtration and washed with diethyl ether to isolated 115 mg of the desired product as an HCl salt, which was then dissolved in 2 ml of DMSO and purified on HPLC: (HPLC condition: Gilson using Trilution software with a Sunfire 5u C18(2) 100A. 50×30.00 mm 5 micron. 7.3-minute run (47 ml/min, 10% ACN/H2O, 0.1% TFA to 35% ACN/H2O, 0.1% TFA) with UV detection at 254 nm). Product fractions were combined and the volume was reduced to remove most of the MeCN. The water left behind was added saturated NaHCO3 and then extracted with EtOAc (3×15 mL). The organic was combined wash with saturated NaCl solution, dried over MgSO4, filtered and concentrated. The material was then transferred into a 40 mL vial with MeCN. Water was added and then it was freeze-dried to give 5-{1-[(2,5-difluorophenyl)acetyl]-2,3-dihydro-1H-indol-5-yl}-7-[2-(4-piperidinyl)ethyl]-7H-pyrrolo[2,3-d]pyrimidin-4-amine (116 mg, 88% yield) as a white solid. LC-MS (ES) m/z=517.6 [M+H]+. 1H NMR (400 MHz, DMSO-d6) δ 8.35 (br. s., 1H), 8.14 (s, 1H), 8.09 (d, J=8.08 Hz, 1H), 7.35 (d, J=4.04 Hz, 2H), 7.15-7.30 (m, 4H), 6.09 (br. s., 2H), 4.29 (t, J=8.34 Hz, 2H), 4.21 (t, J=6.95 Hz, 2H), 3.95 (s, 2H), 3.22-3.30 (m, 4H), 2.77-2.85 (m, 2H), 1.91 (d, J=12.13 Hz, 2H), 1.77 (q, J=6.65 Hz, 2H), 1.47 (br. s., 1H), 1.26-1.38 (m, 2H).

후처리

  1. concentrationThe reaction was concentrated
  2. customthe solid was isolated by filtration
  3. washwashed with diethyl ether

출처 및 근거

ORD 기록
ord-02931446e0fc47a4ba0aab769a7bc271
출처 데이터셋
uspto-grants-2013_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08598156B2

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