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Dimethylamine → HCID 68190287, 화합물

HRID 513779
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HRID 513779 반응식
[CH3:1][NH:2][CH3:3].[Cl:4][C:5]1[CH:6]=[C:7]2[C:16](=[C:17]3[C:22]=1[CH:21]=[CH:20][CH:19]=[N:18]3)[NH:15][S:14](=[O:24])(=[O:23])[C:13]1[C:8]2=[CH:9][C:10]([C:25](O)=[O:26])=[CH:11][CH:12]=1.CCN=C=NCCCN(C)C.Cl.C1C=CC2N(O)N=NC=2C=1>CN(C=O)C.O.C(Cl)Cl>[CH3:1][N:2]([CH3:3])[C:25]([C:10]1[CH:9]=[C:8]2[C:13]([S:14](=[O:24])(=[O:23])[NH:15][C:16]3[C:7]2=[CH:6][C:5]([Cl:4])=[C:22]2[C:17]=3[N:18]=[CH:19][CH:20]=[CH:21]2)=[CH:12][CH:11]=1)=[O:26]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

8

반응물 4

HCID 674DimethylamineHCID 757711-HydroxybenzotriazoleHCID 27239391,3-Propanediamine, N'-(ethylcarbonimidoyl)-N,N-dimethyl-, monohydrochlorideHCID 68190302HCID 68190302, 화합물

생성물 1

HCID 68190287HCID 68190287, 화합물수율 43%

시약·촉매·용매 3

HCID 962
Water
용매
HCID 6228Dimethylformamide용매
HCID 6344Dichloromethane용매

실험 절차

Dimethyl amine (0.2M in THF, 2.77 ml, 0.69 mmol) was added to a solution of 12-chloro-6,6-dioxo-5,6-dihydro-6λ*6*-thia-4,5-diaza-chrysene-9-carboxylic acid 524 (100 mg, 0.27 mmol), EDC.HCl (80 mg, 0.41 mmol), HOBt (56 mg, 0.41 mmol) and TEA (0.12 ml, 0.83 mmol) in DMF (1 ml) and the mixture was stirred at room temperature for 12 h. The mixture was diluted with water and DCM. The organic phase was dried (Na2SO4) and concentrated in vacuo. The crude residue was purified by column chromatography with chloroform/MeOH (95:5) as the eluent to give the title compound (45 mg, 42%).

후처리

  1. dry with materialThe organic phase was dried (Na2SO4)
  2. concentrationconcentrated in vacuo
  3. customThe crude residue was purified by column chromatography with chloroform/MeOH (95:5) as the eluent

출처 및 근거

ORD 기록
ord-88784772e8c94a8ca53af408fee8a95c
출처 데이터셋
uspto-grants-2015_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09102688B2

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