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Hydrochloric Acid → (4-Benzyloxy-phenyl)-(-6-(3-methylisoxazol-5-yl)-quinazolin-4-yl)-amine hydrochloride

HRID 2306737
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HRID 2306737 반응식
[CH2:1]([O:8][C:9]1[CH:14]=[CH:13][C:12]([NH:15][C:16]2[C:25]3[C:20](=[CH:21][CH:22]=[C:23]([C:26]#[CH:27])[CH:24]=3)[N:19]=[CH:18][N:17]=2)=[CH:11][CH:10]=1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[N+:28]([CH2:31][CH3:32])([O-])=[O:29].C1(N=C=O)C=CC=CC=1.[ClH:42]>C(N(CC)CC)C.C(OCC)(=O)C.ClCCl>[ClH:42].[CH2:1]([O:8][C:9]1[CH:10]=[CH:11][C:12]([NH:15][C:16]2[C:25]3[C:20](=[CH:21][CH:22]=[C:23]([C:26]4[O:29][N:28]=[C:31]([CH3:32])[CH:27]=4)[CH:24]=3)[N:19]=[CH:18][N:17]=2)=[CH:13][CH:14]=1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1
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참가 물질

8

반응물 4

HCID 313Hydrochloric AcidHCID 6587NitroethaneHCID 7672Phenyl isocyanateHCID 22609768(4-Benzyloxy-phenyl)(6-ethynylquinazolin-4-yl)-amine

생성물 1

HCID 22609788(4-Benzyloxy-phenyl)-(-6-(3-methylisoxazol-5-yl)-quinazolin-4-yl)-amine hydrochloride수율 11%

시약·촉매·용매 3

HCID 8471
Triethylamine
촉매
HCID 6344Dichloromethane용매
HCID 8857Ethyl Acetate용매

실험 절차

A stirred mixture of (4-benzyloxy-phenyl)-(6-ethynylquinazolin-4-yl)-amine (0.20 g, 0.57 mmol), nitroethane (0.20 g, 2.7 mmol), phenylisocyanate (0.15 ml , 0.164 g, 1.38 mmol), and triethylamine (3 drops) in a mixture of ethyl acetate (10 ml) and dichloromethane (5 ml) was heated at reflux for 18 hours. After cooling the mixture was filtered to remove solid, and the concentrated filtrate was purified by silica gel chromatography, eluting with 50% ethyl acetate/i-hexane. After concentration of the appropriate fractions, the material obtained was treated with methanolic HCl, the solvent was removed in vacuo and the residue was triturated with ether to give the title compound as a yellow solid (0.027 g, 0.061 mmol, 11%); δH [2H6]DMSO 12.0 (1H, s), 9.55 (1H, s), 8.91 (1H, s), 8.48 (1H, d), 8.03 (1H, d), 7.68 (2H, d), 7.32-7.55 (5H, m), 7.22 (1H, s), 7.15 (2H, d), 5.18 (2H, s), 2.35 (3H, s); m/z (M+1+) 409.

후처리

  1. temperaturewas heated
  2. temperatureat reflux for 18 hours
  3. temperatureAfter cooling the mixture
  4. filtrationwas filtered
  5. customto remove solid
  6. customthe concentrated filtrate was purified by silica gel chromatography
  7. washeluting with 50% ethyl acetate/i-hexane
  8. customAfter concentration of the appropriate fractions, the material obtained
  9. customthe solvent was removed in vacuo
  10. customthe residue was triturated with ether

출처 및 근거

ORD 기록
ord-a04e9c4bf03148e58a6760def47031fe
출처 데이터셋
uspto-grants-2004_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06828320B2

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