Dimethylamine → 1-[3,5-dichloro-4-(3,8-dihydroimidazo[4,5-d]dipyrido[2,3-b: 4',3'-f]azepin-2-yl)phenyl]-N,N-dimethylmethanamine

HRID 1043479노트

반응식

HRID 1043479 반응식
[CH3:1][NH:2][CH3:3].[H-].[Na+].[Cl:6][C:7]1[CH:12]=[C:11]([CH2:13]Cl)[CH:10]=[C:9]([Cl:15])[C:8]=1[C:16]1[NH:17][C:18]2[C:24]3[CH:25]=[CH:26][N:27]=[CH:28][C:23]=3[NH:22][C:21]3[N:29]=[CH:30][CH:31]=[CH:32][C:20]=3[C:19]=2[N:33]=1>CN(C)C=O.CO>[Cl:6][C:7]1[CH:12]=[C:11]([CH2:13][N:2]([CH3:3])[CH3:1])[CH:10]=[C:9]([Cl:15])[C:8]=1[C:16]1[NH:17][C:18]2[C:24]3[CH:25]=[CH:26][N:27]=[CH:28][C:23]=3[NH:22][C:21]3[N:29]=[CH:30][CH:31]=[CH:32][C:20]=3[C:19]=2[N:33]=1

참가 물질

6

반응물 3

HCID 674DimethylamineHCID 24758Sodium hydrideHCID 66887168HCID 66887168, 화합물

생성물 1

HCID 160720251-[3,5-dichloro-4-(3,8-dihydroimidazo[4,5-d]dipyrido[2,3-b: 4',3'-f]azepin-2-yl)phenyl]-N,N-dimethylmethanamine수율 31%

시약·촉매·용매 2

HCID 887Methanol용매HCID 6228Dimethylformamide용매

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온도
0 °C

실험 절차

A solution of dimethylamine (23 μL, 2.0 M in tetrahydrofuran) was dissolved in N,N-dimethylformamide (0.5 mL) and cooled to 0° C. Sodium hydride (1.1 mg, 0.05 mmol) was added and the mixture was stirred for 15 minutes. 2-[2,6-dichloro-4-(chloromethyl)phenyl]-3,8-dihydroimidazo[4,5-d]dipyrido[2,3-b:4′,3′-f]azepine (10.0 mg, 0.02 mmol) was added and the mixture was stirred at room temperature for 16 hours. The reaction mixture was diluted with methanol and purified on preparative LCMS at pH 10 to give the desired product (3.2 mg, 31%). LC/MS: 437 (M+H)+.

후처리

  1. stirringthe mixture was stirred at room temperature for 16 hours
  2. custompurified on preparative LCMS at pH 10

출처 및 근거

ORD 기록
ord-81810d57a7544dff82b1d3f3c16505c8
출처 데이터셋
uspto-grants-2013_10
특허 번호
US08563541B2

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