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Hydrochloric Acid → HCID 68657714, 화합물

HRID 1020690
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HRID 1020690 반응식
[ClH:1].CCOCC.[CH3:7][O:8][C:9]1[CH:14]=[CH:13][C:12]([C:15]2[CH:20]=[CH:19][N:18]([C:21]3[CH:22]=[CH:23][C:24]4[C:25]5[CH2:34][NH:33][CH2:32][CH2:31][C:26]=5[N:27]([CH3:30])[C:28]=4[CH:29]=3)[C:17](=[O:35])[CH:16]=2)=[C:11]([CH3:36])[CH:10]=1>C(Cl)Cl>[ClH:1].[CH3:7][O:8][C:9]1[CH:14]=[CH:13][C:12]([C:15]2[CH:20]=[CH:19][N:18]([C:21]3[CH:22]=[CH:23][C:24]4[C:25]5[CH2:34][NH:33][CH2:32][CH2:31][C:26]=5[N:27]([CH3:30])[C:28]=4[CH:29]=3)[C:17](=[O:35])[CH:16]=2)=[C:11]([CH3:36])[CH:10]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 313Hydrochloric AcidHCID 3283Diethyl EtherHCID 52947558HCID 52947558, 화합물

생성물 1

HCID 68657714HCID 68657714, 화합물수율 85%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

2 N HCl in Et2O (0.40 mL, 0.80 mmol) was added to a solution of 4-(4-methoxy-2-methylphenyl)-1-(5-methyl-2,3,4,5-tetrahydro-1H-pyrido[4,3-b]indol-7-yl)pyridin-2(1H)-one (0.16 g, 0.40 mmol) in CH2Cl2 (1.5 mL), and the solution was stirred at ambient temperature for 1 h under N2. The solids were collected by filtration, washed with Et2O and dried to yield the title compound (0.15 g, 85%) as an off-white powder: 1H NMR (500 MHz, DMSO-d6) δ 9.39 (br s, 2H), 7.67 (d, J=7.0 Hz, 1H), 7.59 (d, J=8.0 Hz, 1H), 7.27 (d, J=2.0 Hz, 1H), 7.25 (d, J=8.5 Hz, 1H), 7.10 (dd, J=8.5, 2.0 Hz, 1H), 6.92 (d, J=2.5 Hz, 1H), 6.88 (dd, J=8.0, 2.5 Hz, 1H), 6.37 (d, J=2.0 Hz, 1H), 6.34 (dd, J=7.0, 2.0 Hz, 1H), 4.36-4.34 (m, 2H), 3.79 (s, 3H), 3.71 (s, 3H), 3.53-3.52 (m, 2H), 3.10 (t, J=6.0 Hz, 2H), 2.35 (s, 3H); ESI MS m/z 400 [M+H]; HPLC (Method A) 95.8% (AUC), tR=14.5 min.

후처리

  1. filtrationThe solids were collected by filtration
  2. washwashed with Et2O
  3. customdried

출처 및 근거

ORD 기록
ord-4b85a18432e543559fa1c5fd09453672
출처 데이터셋
uspto-grants-2014_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08716308B2

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