Cyclopropylamine → HCID 58930836, 화합물

HRID 387940

반응식

HRID 387940 반응식
[F:1][C:2]1[CH:33]=[CH:32][C:5]([NH:6][C:7]([NH:9][C:10]2[CH:31]=[CH:30][C:13]([O:14][C:15]3[C:24]4[C:19](=[CH:20][C:21]([O:28][CH3:29])=[C:22]([C:25](O)=[O:26])[CH:23]=4)[N:18]=[CH:17][CH:16]=3)=[CH:12][CH:11]=2)=[O:8])=[CH:4][CH:3]=1.Cl.C(N=C=N[CH2:40][CH2:41][CH2:42][N:43](CC)CC)C.O.ON1C2C=CC=CC=2N=N1.C1(N)CC1>CN(C)C=O.O.C(OCC)(=O)C.C(N(CC)CC)C>[CH:42]1([NH:43][C:25]([C:22]2[CH:23]=[C:24]3[C:19](=[CH:20][C:21]=2[O:28][CH3:29])[N:18]=[CH:17][CH:16]=[C:15]3[O:14][C:13]2[CH:30]=[CH:31][C:10]([NH:9][C:7]([NH:6][C:5]3[CH:32]=[CH:33][C:2]([F:1])=[CH:3][CH:4]=3)=[O:8])=[CH:11][CH:12]=2)=[O:26])[CH2:40][CH2:41]1

참가 물질

9

반응물 4

HCID 69828CyclopropylamineHCID 27960291-Hydroxybenzotriazole hydrateHCID 99645121-(3-Diethylaminopropyl)-3-ethylcarbodiimide hydrochlorideHCID 229363504-(4-(((4-Fluoroanilino)carbonyl)amino)phenoxy)-7-methoxy-6-quinolinecarboxylic acid

생성물 1

HCID 58930836HCID 58930836, 화합물수율 44.5%

시약·촉매·용매 4

HCID 962Water용매HCID 6228Dimethylformamide용매HCID 8471Triethylamine용매HCID 8857Ethyl Acetate용매

실험 절차

After dissolving the N-[4-(6-carboxy-7-methoxy-4-quinolyl)oxyphenyl]-N′-(4-fluorophenyl)urea (60 mg) synthesized in Example 341 in dimethylformamide (1.5 ml), there were added 1-ethyl-3-(3-diethylaminopropyl)-carbodiimide hydrochloride (39 mg), 1-hydroxy-1H-benzotriazole monohydrate (31 mg), triethylamine (30 μl) and cyclopropylamine (0.05 ml) and the mixture was stirred overnight at room temperature. The reaction solution was distributed between ethyl acetate and water, and the organic layer was washed with water and then dried over anhydrous sodium sulfate. After distilling off the solvent, crystals were precipitated with ethyl acetate, filtered out and dried under reduced pressure to obtain the title compound (29 mg) as white crystals.

후처리

  1. washthe organic layer was washed with water
  2. dry with materialdried over anhydrous sodium sulfate
  3. distillationAfter distilling off the solvent, crystals
  4. customwere precipitated with ethyl acetate
  5. filtrationfiltered out
  6. customdried under reduced pressure

출처 및 근거

ORD 기록
ord-3420ff75cd274140a16e1c02037ed533
출처 데이터셋
uspto-grants-2013_02
특허 번호
US08372981B2

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