1-Hydroxybenzotriazole → HCID 67180248, 화합물

HRID 1863994

반응식

HRID 1863994 반응식
[F:1][C:2]1[CH:7]=[CH:6][C:5]([C:8]2[C:13]3[CH2:14][NH:15][CH2:16][CH2:17][O:18][C:12]=3[N:11]=[CH:10][CH:9]=2)=[CH:4][CH:3]=1.ON1C2C=CC=CC=2N=N1.[C:29]([O:33][C:34]([NH:36][CH2:37][C:38]1[CH:39]=[C:40]([CH:44]=[CH:45][CH:46]=1)[C:41](O)=[O:42])=[O:35])([CH3:32])([CH3:31])[CH3:30].Cl.C(N=C=NCCCN(C)C)C>C(#N)C.C(OCC)(=O)C.C(N(CC)CC)C>[F:1][C:2]1[CH:3]=[CH:4][C:5]([C:8]2[C:13]3[CH2:14][N:15]([C:41]([C:40]4[CH:39]=[C:38]([CH:46]=[CH:45][CH:44]=4)[CH2:37][NH:36][C:34](=[O:35])[O:33][C:29]([CH3:31])([CH3:32])[CH3:30])=[O:42])[CH2:16][CH2:17][O:18][C:12]=3[N:11]=[CH:10][CH:9]=2)=[CH:6][CH:7]=1

참가 물질

8

반응물 4

HCID 757711-HydroxybenzotriazoleHCID 27239391,3-Propanediamine, N'-(ethylcarbonimidoyl)-N,N-dimethyl-, monohydrochlorideHCID 27559293-(((tert-Butoxycarbonyl)amino)methyl)benzoic acidHCID 690781546-(4-Fluorophenyl)-2,3,4,5-tetrahydropyrido[3,2-f][1,4]oxazepine

생성물 1

HCID 67180248HCID 67180248, 화합물수율 89.8%

시약·촉매·용매 3

HCID 6342Acetonitrile용매HCID 8471Triethylamine용매HCID 8857Ethyl Acetate용매

실험 절차

To a solution of 6-(4-fluorophenyl)-2,3,4,5-tetrahydropyrido[3,2-f][1,4]oxazepine (0.20 g) obtained in Reference Example 13C, 1-hydroxy-1H-benzotriazole (0.15 g), triethylamine (0.083 g) and 3-(tert-butoxycarbonylaminomethyl)benzoic acid (0.205 g) in acetonitrile (10 ml) was added 1-ethyl-3-(3-dimethylaminopropyl)carbodiimide hydrochloride (0.314 g), and the mixture was stirred at room temperature for 20 hrs. Ethyl acetate was added to the reaction mixture, and the mixture was washed with water, and dried over anhydrous magnesium sulfate. The solvent was evaporated and the residue was purified by silica gel column chromatography to give the title compound (0.35 g) as a colorless amorphous powder.

후처리

  1. washthe mixture was washed with water
  2. dry with materialdried over anhydrous magnesium sulfate
  3. customThe solvent was evaporated
  4. customthe residue was purified by silica gel column chromatography

출처 및 근거

ORD 기록
ord-43c476ba5ce64a4b9cf6588523737150
출처 데이터셋
uspto-grants-2009_12
특허 번호
US07625887B2

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