Methyl iodide → HCID 19756360, 화합물

HRID 1587832노트

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HRID 1587832 반응식
[H-].[Na+].[CH2:3]([C:5]1[CH:14]=[C:13]([O:15][CH2:16][C:17]2[CH:22]=[CH:21][C:20]([C:23]3[CH:28]=[CH:27][CH:26]=[CH:25][C:24]=3[C:29]3[N:30]=[N:31][N:32]([C:34]([C:47]4[CH:52]=[CH:51][CH:50]=[CH:49][CH:48]=4)([C:41]4[CH:46]=[CH:45][CH:44]=[CH:43][CH:42]=4)[C:35]4[CH:40]=[CH:39][CH:38]=[CH:37][CH:36]=4)[N:33]=3)=[CH:19][CH:18]=2)[C:12]2[C:7](=[CH:8][CH:9]=[C:10]([O:53][CH2:54][CH2:55][OH:56])[N:11]=2)[N:6]=1)[CH3:4].[H][H].CI.C1C[O:64][CH2:63][CH2:62]1>O>[CH2:3]([C:5]1[CH:14]=[C:13]([O:15][CH2:16][C:17]2[CH:18]=[CH:19][C:20]([C:23]3[CH:28]=[CH:27][CH:26]=[CH:25][C:24]=3[C:29]3[N:30]=[N:31][N:32]([C:34]([C:47]4[CH:48]=[CH:49][CH:50]=[CH:51][CH:52]=4)([C:41]4[CH:42]=[CH:43][CH:44]=[CH:45][CH:46]=4)[C:35]4[CH:40]=[CH:39][CH:38]=[CH:37][CH:36]=4)[N:33]=3)=[CH:21][CH:22]=2)[C:12]2[C:7](=[CH:8][CH:9]=[C:10]([O:53][CH2:54][C:55]([O:64][CH2:63][CH3:62])=[O:56])[N:11]=2)[N:6]=1)[CH3:4]

참가 물질

7

반응물 5

HCID 6328Methyl iodideHCID 8028TetrahydrofuranHCID 24758Sodium hydrideHCID 19756350HCID 19756350, 화합물HCID 178418361HCID 178418361, 화합물

생성물 1

HCID 19756360HCID 19756360, 화합물

시약·촉매·용매 1

HCID 962Water용매

실험 절차

Sodium hydride (60% dispersion in mineral oil, 62 mg) was added in a solution of 2-ethyl-6-(2-hydroxyethoxy)-4-[(2'-(2-triphenylmethyl-2H-tetrazol-5-yl)biphenyl-4-yl)methoxy]-1,5-naphthyridine (1.0 g) in THF (10 ml). The mixture was stirred until evolution of hydrogen had ceased and then methyl iodide (0.09 ml) was added. The solution was left to stand for 72 hours and then water (30 ml) was added. The mixture was extracted with ether (2×20 ml) and the combined extracts were dried (MgSO4). Volatile material was removed by evaporation and the residue was triturated with hexane to give 2-ethyl-6-(2-methoxyethoxy)-4-[(2'-(2-triphenylmethyl-2H-tetrazol-5-yl)biphenyl-4-yl)methoxy]-1,5-naphthyridine (A) (0.86 g), as a foam; NMR (d6 -DMSO): 1.3(t, 3H), 2.8(q, 2H), 3.25(s, 3H), 3.6-3.7(m, 2H), 4.45-4.55(m, 2H), 5.4(s, 2H), 6.8-6.9(m, 6H), 7.1-7.7(complex m, 18H), 7.8(dd, 1H), 8.15(d, 1H).

후처리

  1. waitThe solution was left
  2. extractionThe mixture was extracted with ether (2×20 ml)
  3. dry with materialthe combined extracts were dried (MgSO4)
  4. customVolatile material was removed by evaporation
  5. customthe residue was triturated with hexane

출처 및 근거

ORD 기록
ord-57fcaaabc29c4f6ab879df9c4106f3c2
출처 데이터셋
uspto-grants-1993_06
특허 번호
US05219863

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