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Triethylamine → 1-(4-(4-chlorobenzyl)-1-(7H-pyrrolo(2,3-d)pyrimidin-4-yl)piperidin-4-yl)methanamine

HRID 2405985
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HRID 2405985 반응식
Cl.[Cl:2][C:3]1[CH:17]=[CH:16][C:6]([CH2:7][C:8]2([CH2:14][NH2:15])[CH2:13][CH2:12][NH:11][CH2:10][CH2:9]2)=[CH:5][CH:4]=1.Cl[C:19]1[C:20]2[CH:27]=[CH:26][NH:25][C:21]=2[N:22]=[CH:23][N:24]=1.C(N(CC)CC)C>C(O)CCC>[Cl:2][C:3]1[CH:17]=[CH:16][C:6]([CH2:7][C:8]2([CH2:14][NH2:15])[CH2:13][CH2:12][N:11]([C:19]3[C:20]4[CH:27]=[CH:26][NH:25][C:21]=4[N:22]=[CH:23][N:24]=3)[CH2:10][CH2:9]2)=[CH:5][CH:4]=1
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참가 물질

5

반응물 3

HCID 8471TriethylamineHCID 53566827H-Pyrrolo(2,3-d)pyrimidine, 4-chloro-HCID 66873182885500-40-3

생성물 1

HCID 116961131-(4-(4-chlorobenzyl)-1-(7H-pyrrolo(2,3-d)pyrimidin-4-yl)piperidin-4-yl)methanamine수율 56%

시약·촉매·용매 1

HCID 2631-Butanol용매

실험 절차

A solution of C-[4-(4-chlorobenzyl)piperidin-4-yl]methyl amine hydrochloride (0.063 g, 0.2016 mmol), 4-chloro-7H-pyrrolo[2,3-d]pyrimidine (0.031 g, 0.2016 mmol) and triethylamine (0.140 ml, 1.0079 mmol) in n-butanol (2.0 ml) was heated to 100° C. for 24 hours. Concentration and purification by SCX-2 Isolute column (2 g), eluting with 1M NH3/MeOH, followed by silica column chromatography (15% methanol in DCM) gave a white solid (0.040 g, 56%). LC-MS (LCT2) m/z 356 [M+H+], Rt 2.97 min.

후처리

  1. concentrationConcentration and purification by SCX-2 Isolute column (2 g)
  2. washeluting with 1M NH3/MeOH

출처 및 근거

ORD 기록
ord-02879415fd9343948b94740bdc5da53b
출처 데이터셋
uspto-grants-2014_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08809336B2

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