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N-BOC-ethylenediamine → HCID 10048021, 화합물

HRID 1271884
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HRID 1271884 반응식
C(O[C:6](=O)[NH:7][CH2:8][CH2:9][NH:10][CH:11]([C:14]1[N:23]([CH2:24][C:25]2[CH:30]=[CH:29][CH:28]=[CH:27][CH:26]=2)[C:22](=[O:31])[C:21]2[C:16](=[CH:17][C:18]([Cl:32])=[CH:19][CH:20]=2)[N:15]=1)[CH2:12][CH3:13])(C)(C)C.C(N1[C:50](=[O:51])[C:49]2C(=CC(Cl)=CC=2)N=C1C(Br)CC)C1C=CC=CC=1.C(OC(=O)NCCN)(C)(C)C.C(=O)(O)[O-].[Na+]>CCO>[CH2:24]([N:23]1[C:22](=[O:31])[C:21]2[C:16](=[CH:17][C:18]([Cl:32])=[CH:19][CH:20]=2)[N:15]=[C:14]1[CH:11]([N:10]1[C:50](=[O:51])[CH2:49][CH2:6][NH:7][CH2:8][CH2:9]1)[CH2:12][CH3:13])[C:25]1[CH:26]=[CH:27][CH:28]=[CH:29][CH:30]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 187201N-BOC-ethylenediamineHCID 516892Sodium BicarbonateHCID 184550303-Benzyl-2-(1-bromopropyl)-7-chloroquinazolin-4(3H)-oneHCID 69478431HCID 69478431, 화합물

생성물 1

HCID 10048021HCID 10048021, 화합물

시약·촉매·용매 1

HCID 702Ethanol
용매

실험 절차

Preparation of {2-[1-(3-benzyl-7-chloro-4-oxo-3,4-dihydro-quinazolin-2-yl)-propylamino]-ethyl}-carbamic acid tert-butyl ester: A mixture of 3-benzyl-2-(1-bromo-propyl)-7-chloro-3H-quinazolin-4-one (3.9 g, 10 mmol) (WO 0130768), (2-amino-ethyl)-carbamic acid tert-butyl ester (2.40 g, 15 mmol) and sodium bicarbonate (1.26 g, 15 mmol) in EtOH (50 mL) was refluxed overnight. The salts were removed by filtration and the filtrate was concentrated to dryness. The residue which remained was purified by flash chromatography on silica gel (10–15% EtOH in hexane) to give the title compound (2.90 g) as a white solid: MS (ES) m/e 471.2 (M+H)+.

후처리

  1. temperaturewas refluxed overnight
  2. customThe salts were removed by filtration
  3. concentrationthe filtrate was concentrated to dryness
  4. customThe residue which remained was purified by flash chromatography on silica gel (10–15% EtOH in hexane)

출처 및 근거

ORD 기록
ord-1b21b5a7e580453d8e1ea1f13963e52f
출처 데이터셋
uspto-grants-2007_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07208487B2

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