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HCID 67208015, 화합물 → 7-(3,5-dimethyl-4-isoxazolyl)-N4-(phenylmethyl)-3,4-quinolinediamine

HRID 1042985
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HRID 1042985 반응식
[C:1]([C:5]1[CH:10]=[CH:9][CH:8]=C[C:6]=1[NH:11][C:12]1[C:21]2[C:16](=[CH:17][C:18]([C:22]3[C:23]([CH3:28])=[N:24][O:25][C:26]=3[CH3:27])=[CH:19][CH:20]=2)[N:15]=[CH:14][C:13]=1[N+:29]([O-])=O)(C)(C)[CH3:2]>C(O)C.C1COCC1>[CH3:28][C:23]1[C:22]([C:18]2[CH:17]=[C:16]3[C:21]([C:12]([NH:11][CH2:6][C:5]4[CH:1]=[CH:2][CH:8]=[CH:9][CH:10]=4)=[C:13]([NH2:29])[CH:14]=[N:15]3)=[CH:20][CH:19]=2)=[C:26]([CH3:27])[O:25][N:24]=1
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참가 물질

4

반응물 1

HCID 67208015HCID 67208015, 화합물2회

생성물 1

HCID 672063207-(3,5-dimethyl-4-isoxazolyl)-N4-(phenylmethyl)-3,4-quinolinediamine수율 100.6%

시약·촉매·용매 2

HCID 702Ethanol용매HCID 8028Tetrahydrofuran용매

실험 절차

To a solution of N-[2-(tert-butyl)phenyl]-7-(3,5-dimethyl-4-isoxazolyl)-3-nitro-4-quinolinamine (see Intermediate 19, 2.4 g, 5.77 mmol) in a mixture of ethanol (60 ml) and THF (20 ml), was added SnCl2,2H2O (7.81 g, 34.6 mmol). The reaction mixture was refluxed for 3 h and then concentrated to dryness. The resulting residue was poured into aqueous sodium hydroxide. The organic phase was extracted with EtOAc, washed with water, dried and concentrated to give the title compound as a yellow solid (2 g, 71%). [APCI-MS] m/z: 387 MH+, Rt 3.37 min.

후처리

  1. temperatureThe reaction mixture was refluxed for 3 h
  2. concentrationconcentrated to dryness
  3. additionThe resulting residue was poured into aqueous sodium hydroxide
  4. extractionThe organic phase was extracted with EtOAc
  5. washwashed with water
  6. customdried
  7. concentrationconcentrated

출처 및 근거

ORD 기록
ord-62fe508c153e48e19212cdace83a1714
출처 데이터셋
uspto-grants-2013_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08557984B2

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