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Hydrochloric Acid → HCID 178421995, 화합물

HRID 487374
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HRID 487374 반응식
[ClH:1].[CH3:2][C:3]1[N:12]=[C:11]([CH3:13])[CH:10]=[C:9]2[C:4]=1[CH:5]=[CH:6][C:7](=[O:51])[N:8]2[CH2:14][C:15]1[CH:20]=[CH:19][C:18]([C:21]2[CH:26]=[CH:25][CH:24]=[CH:23][C:22]=2[C:27]2[N:28]=[N:29][N:30](C(C3C=CC=CC=3)(C3C=CC=CC=3)C3C=CC=CC=3)[N:31]=2)=[CH:17][CH:16]=1>ClCCl.CO>[ClH:1].[CH3:2][C:3]1[N:12]=[C:11]([CH3:13])[CH:10]=[C:9]2[C:4]=1[CH:5]=[CH:6][C:7](=[O:51])[N:8]2[CH2:14][C:15]1[CH:20]=[CH:19][C:18]([C:21]2[CH:26]=[CH:25][CH:24]=[CH:23][C:22]=2[C:27]2[NH:28][N:29]=[N:30][N:31]=2)=[CH:17][CH:16]=1
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4

반응물 2

HCID 313Hydrochloric AcidHCID 190937065,7-dimethyl-1-[(2'-(2-triphenylmethyl-2H-tetrazol-5-yl)biphenyl-4-yl)methyl]-1,6-naphthyridin-2(1H)-one

생성물 1

HCID 178421995HCID 178421995, 화합물

시약·촉매·용매 1

HCID 21226129Dichloromethane methanol용매

실험 절차

Concentrated hydrochloric acid (0.3 ml) was added to a solution of 5,7-dimethyl-1-[(2'-(2-triphenylmethyl-2H-tetrazol-5-yl)biphenyl-4-yl)methyl]-1,6-naphthyridin-2(1H)-one (280 mg) (A) in dichloromethane/methanol (4 ml) (3:1 v/v) and the mixture was stirred for 30 minutes. Volatile material was removed by evaporation and the residue was stirred with ether. The insoluble solid was collected by filtration and recrystallised from ethanol/methanol (1:1 v/v) to give 5,7-dimethyl-1-[(2'-(1H-tetrazol-5-yl)biphenyl-4-yl)methyl]-1,6-naphthyridin-2(1H)-one hydrochloride (105 mg), as a solid, m.p. 278°-280° C. (decomposition); NMR (d6 -DMSO): 2.68(s,3H), 2.96(s,3H), 5.51(s,2H), 6.94(d,1H), 7.05(d,2H), 7.17(d,2H), 7.45-7.71(m,5H), 8.31(d,1H); mass spectrum (positive fast atom bombardment (+ve FAB), DMSO/methanol/nitrobenzyl alcohol(NBA)): 409(M+H)+ ; microanalysis, found: C, 64.1; H, 4.6; N, 18.7%; C24H20N6O.HCl.0.2H2O requires: C,64.1; H,4.8; N,18.7%.

후처리

  1. customVolatile material was removed by evaporation
  2. stirringthe residue was stirred with ether
  3. filtrationThe insoluble solid was collected by filtration
  4. customrecrystallised from ethanol/methanol (1:1 v/v)

출처 및 근거

ORD 기록
ord-5bab83c0e57742a8b2e27bd18f5207e2
출처 데이터셋
uspto-grants-1994_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05294620

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