Water → HCID 19756360, 화합물

HRID 1587837노트

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HRID 1587837 반응식
[CH2:1]([O:3][C:4]([CH:6]([O:8][C:9]1[N:10]=[C:11]2[C:16](=[CH:17][CH:18]=1)[N:15]=[C:14]([CH2:19][CH3:20])[CH:13]=[C:12]2[O:21][CH2:22][C:23]1[CH:28]=[CH:27][C:26]([C:29]2[CH:34]=[CH:33][CH:32]=[CH:31][C:30]=2[C:35]2[N:36]=[N:37][N:38]([C:40]([C:53]3[CH:58]=[CH:57][CH:56]=[CH:55][CH:54]=3)([C:47]3[CH:52]=[CH:51][CH:50]=[CH:49][CH:48]=3)[C:41]3[CH:46]=[CH:45][CH:44]=[CH:43][CH:42]=3)[N:39]=2)=[CH:25][CH:24]=1)C)=[O:5])[CH3:2].[H-].[Al+3].[Li+].[H-].[H-].[H-].O.[OH-].[Na+]>C1COCC1>[CH2:19]([C:14]1[CH:13]=[C:12]([O:21][CH2:22][C:23]2[CH:24]=[CH:25][C:26]([C:29]3[CH:34]=[CH:33][CH:32]=[CH:31][C:30]=3[C:35]3[N:36]=[N:37][N:38]([C:40]([C:53]4[CH:58]=[CH:57][CH:56]=[CH:55][CH:54]=4)([C:47]4[CH:48]=[CH:49][CH:50]=[CH:51][CH:52]=4)[C:41]4[CH:46]=[CH:45][CH:44]=[CH:43][CH:42]=4)[N:39]=3)=[CH:27][CH:28]=2)[C:11]2[C:16](=[CH:17][CH:18]=[C:9]([O:8][CH2:6][C:4]([O:3][CH2:1][CH3:2])=[O:5])[N:10]=2)[N:15]=1)[CH3:20]

참가 물질

6

반응물 4

HCID 962Water2회HCID 14798Sodium HydroxideHCID 19756353HCID 19756353, 화합물HCID 21226445Aluminium lithium hydride

생성물 1

HCID 19756360HCID 19756360, 화합물수율 90.7%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매2회

실험 절차

A solution of 6-[1-(ethoxycarbonyl)ethoxy]-2-ethyl-4-[(2'-(2-triphenylmethyl-2H-tetrazol-5-yl)biphenyl-4-yl)methoxy]-1,5-naphthyridine (1.0 g) in THF (8 ml) was added to a stirred suspension of lithium aluminium hydride (100 mg) in THF (5 ml) at 0° C. The mixture was allowed to warm to ambient temperature and then stirred for 20 hours. Water (0.1 ml), 15% w/v sodium hydroxide solution (0.1 ml) and water (0.3 ml) were added and the mixture was stirred for 30 minutes. The insoluble solid was removed by filtration and the filtrate was concentrated by evaporation. The residue was triturated with ether to give 2-ethyl-6-(1-hydroxy-2-propoxy)-4-[(2'-(2-triphenylmethyl-2H-tetrazol-5-yl)biphenyl-4-yl)methoxy]-1,5-naphthyridine (A) (0.89 g), m.p. 146°-150° C.; NMR (d6 -DMSO); 1.25-1.35(m, 6H), 2.8(q, 2H), 3.35-3.45(m, 1H), 3.6(s, 2H), 5.4(s, 2H), 6.8-6.9(m, 6H), 7.05-7.15(m, 3H), 7.2-7.4(m, 10H), 7.45-7.6(m, 5H), 7.8(dd, 1H), 8.1(d, 1H).

후처리

  1. additionwere added
  2. stirringthe mixture was stirred for 30 minutes
  3. customThe insoluble solid was removed by filtration
  4. concentrationthe filtrate was concentrated by evaporation
  5. customThe residue was triturated with ether

출처 및 근거

ORD 기록
ord-a702a0267ff246fe8295aa8a5329a560
출처 데이터셋
uspto-grants-1993_06
특허 번호
US05219863

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