Triethylamine → 7-(3,5-Dimethylisoxazol-4-yl)-6-methoxy-N-(1-methoxypropan-2-yl)-3-nitroquinolin-4-amine

HRID 81986

반응식

HRID 81986 반응식
[CH3:1][O:2][CH2:3][CH:4]([NH2:6])[CH3:5].Cl[C:8]1[C:17]2[C:12](=[CH:13][C:14]([C:20]3[C:21]([CH3:26])=[N:22][O:23][C:24]=3[CH3:25])=[C:15]([O:18][CH3:19])[CH:16]=2)[N:11]=[CH:10][C:9]=1[N+:27]([O-:29])=[O:28].C(N(CC)CC)C>CN1C(=O)CCC1.O>[CH3:26][C:21]1[C:20]([C:14]2[CH:13]=[C:12]3[C:17]([C:8]([NH:6][CH:4]([CH3:5])[CH2:3][O:2][CH3:1])=[C:9]([N+:27]([O-:29])=[O:28])[CH:10]=[N:11]3)=[CH:16][C:15]=2[O:18][CH3:19])=[C:24]([CH3:25])[O:23][N:22]=1

참가 물질

6

반응물 3

HCID 8471TriethylamineHCID 123458MethoxyisopropylamineHCID 574655804-(4-Chloro-6-methoxy-3-nitroquinolin-7-yl)-3,5-dimethylisoxazole

생성물 1

HCID 709805047-(3,5-Dimethylisoxazol-4-yl)-6-methoxy-N-(1-methoxypropan-2-yl)-3-nitroquinolin-4-amine수율 93%

시약·촉매·용매 2

HCID 962Water용매HCID 13387N-methyl-2-pyrrolidone용매

실험 절차

1-(Methyloxy)-2-propanamine (0.35 g) and 4-chloro-7-(3,5-dimethyl-4-isoxazolyl)-6-(methyloxy)-3-nitroquinoline (for a preparation see Intermediate 8) (0.74 g, 2.217 mmol) were dissolved in a mixture of triethylamine (0.30 ml, 2.2 mmol) and NMP (3 ml) and the solution was allowed to stand for 30 min at room temperature, then diluted with water (20 ml) and the resulting suspension stirred for 20 min, then filtered and the resulting solid washed with water (10 ml) and dried in the vacuum oven at 50° C. to give the title compound as bright yellow solid. (0.80 g, 2.070 mmol, 93% yield). LCMS (formate) Rt 0.97 MH+ 387

후처리

  1. filtrationfiltered
  2. washthe resulting solid washed with water (10 ml)
  3. customdried in the vacuum oven at 50° C.

출처 및 근거

ORD 기록
ord-f38cf3b8a8294bdb8d82abf63fdbd1ec
출처 데이터셋
uspto-grants-2014_09
특허 번호
US08846709B2

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